CN104874196B - A kind of method processing sodium and ammonium acetate salt-diazonium Organic substance-methanol-water mixed solution - Google Patents
A kind of method processing sodium and ammonium acetate salt-diazonium Organic substance-methanol-water mixed solution Download PDFInfo
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Abstract
A kind of continuous external circulation reaction side line rectification and liquid-liquid extraction combination process sodium and ammonium acetate salt, diazonium Organic substance, methanol and the method for water mixed solution, raw material mixed liquor adds reaction side line rectifying column with alkali liquor after mixing, tower bottoms outer circulation, reacted side line rectification ammonium salt therein is converted into sodium salt, and isolate tail gas ammonia and methanol, obtained containing sodium acetate by dust-settling compartment, diazonium Organic substance and aqueous mixtures, again by this mixture with hexamethylene for extractant liquid-liquid extraction, obtain sodium acetate aqueous solution and organic facies, sodium acetate aqueous solution obtains sodium acetate through evaporation, organic facies reclaims diazonium Organic substance through flash distillation, after separation, extractant recycles；Tail gas is sulfuric acid-treated simultaneously obtains ammonium sulfate.The inventive method respectively obtains technical grade acetic acid sodium, more than 95wt% methanol, more than 97wt% diazonium Organic substance and ammonium sulfate, and after separation, the COD of water is less than 1000PPM.It is simple that the present invention has processing step, the advantage that separation process energy consumption is low.
Description
Technical field
The present invention relates to a kind of multicomponent mixture treatment of Organic Wastewater and the technique of separation, be specifically related to a kind of continuous external circulation reaction
Rectification and liquid-liquid extraction combination process sodium and ammonium acetate salt, diazonium Organic substance, methanol and the separation method of water mixed solution.
Background technology
Pymetrozine is novel heterocyclic efficient selective insecticide, has the strongest interior absorption, can be the most absorbed by crops,
Each position of crop is spread to by Uptake and translocation effect.Exactly because the mechanism of action that pymetrozine is unique so that it is there is height
Selectivity (only the most effective to sucking mouthpart insecticide), to mammal, birds, fish and shrimp, Apis, non-target arthropod
Deng there being good safety.
In pymetrozine production process, produce a large amount of waste water, mainly comprise sodium and ammonium acetate salt, diazonium Organic substance and methanol.
Recovery and processing method for above-mentioned salt-containing organic wastewater mainly have physico-chemical process, biochemical process and chemical hydrolysis the most both at home and abroad.
Use biochemical process and chemical hydrolysis all can destroy effective ingredient in waste water.It is not thorough that biochemical process processes time length, degraded, this
Outward, diazonium Organic substance can make microorganism be poisoned, and biological treatment causes extreme shock, and processing cost is high；Chemical method does not reach
To reclaiming salt and the purpose of methanol, easily cause secondary pollution.
Such as take effectively to process and separation method to above-mentioned mixed liquor, be possible not only to obtain the high sodium acetate of added value and methanol,
Reach to process the purpose of waste water simultaneously, significantly reduce processing procedure cost, obtain preferable economic benefit.Use conventional distil-lation
Method processes above-mentioned salt-containing organic wastewater, needs repeatedly to distill, and forms saliferous organic solid castoff after process, giving up after process
Water COD reaches 40000PPM, it is still necessary to carrying out biochemical treatment, processing procedure expense, energy consumption are higher.
Summary of the invention
It is an object of the invention to provide a kind of continuous external circulation reaction side line rectification and liquid-liquid extraction combination processes sodium and ammonium acetic acid
Salt, diazonium Organic substance, methanol and the technique of water mixed solution, be first converted into sodium salt through primary first-order equation side line rectification by ammonium salt,
And isolate tail gas ammonia and methanol, obtain containing sodium acetate, diazonium Organic substance and aqueous mixtures again through liquid-liquid extraction, separate
To sodium acetate aqueous solution and the organic facies comprising diazonium Organic substance, extractant, sodium acetate aqueous solution obtains finely through evaporation process
Chemicals sodium acetate, organic facies is through flash separation extractant recyclable diazonium Organic substance, and extractant can recycle；Tail gas
Ammonia processes through Waste Sulfuric Acid and obtains ammonium sulfate.Said process respectively obtains sodium acetate, methanol, diazonium Organic substance and ammonium sulfate, point
It is less than 1000PPM from the COD of rear water, industrial wastewater treatment system can be entered；Compared with traditional handicraft, the present invention has work
Skill step is simple, the advantage that separation process energy consumption is low.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of continuous external circulation reaction side line rectification and liquid-liquid extraction combination process sodium and ammonium acetate salt, diazonium Organic substance, methanol
With the method for water mixed solution, comprise the following steps:
1) from reaction after raw material sodium and ammonium acetate salt, diazonium Organic substance, methanol and water mixed solution are mixed by reaction ratio with alkali liquor
Side line rectifying column middle and lower part material inlet adds, and reaction side line tower bottom of rectifying tower liquid is by outer circulation pump pump to material inlet
The recycle feed mouth of side carries out outer circulation, reacted side line rectification, and the ammonium salt in material liquid is converted into sodium salt, reacts side line
Rectification bottom discharge is to liquid reducing chamber, and liquid reducing chamber discharging is containing sodium acetate, diazonium Organic substance and aqueous mixtures, reacts side line rectification
Tower side line, tower top respectively obtain more than 95wt% methanol and tail gas ammonia；
2) multistage liquid-liquid extraction tower is entered containing sodium acetate, diazonium Organic substance and aqueous mixtures, with hexamethylene as extractant, through many
Stage countercurrent liquid-liquid extraction, at the bottom of tower, tower top respectively obtain sodium acetate aqueous solution and comprise the organic facies of diazonium Organic substance, extractant,
Obtaining 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 of generation contains
Amount is less than 0.1wt%；
3) multistage liquid-liquid extraction tower top is the organic facies being mainly made up of extractant and diazonium Organic substance, processes through flash column, tower
Top is extracted agent, is recycled to multistage liquid liquid counter-current extraction tower and recycles, obtains content >=97wt% diazonium Organic substance at the bottom of tower.
The inventive method establishes the technique that a kind of successive reaction side line rectification and liquid-liquid extraction combine, for sodium and ammonium acetate salt,
Diazonium Organic substance, methanol and water mixed solution, through primary first-order equation side line rectification, can be converted into sodium salt by ammonium salt therein, and
Isolate tail gas ammonia and methanol, obtain containing sodium acetate, diazonium Organic substance and aqueous mixtures, then it is organic to contain sodium acetate, diazonium
Thing and aqueous mixtures with hexamethylene for extractant through liquid-liquid extraction, respectively obtain sodium acetate aqueous solution and comprise diazonium Organic substance,
The organic facies of extractant, sodium acetate aqueous solution obtains sodium acetate through evaporation process, and organic facies is recyclable through flash separation extractant
Diazonium organic matter circling uses, and the extractant after separation can recycle；Meanwhile, the methanol respectively obtained and tail gas ammonia,
Methanol recycles as solvent, and tail gas ammonia processes through Waste Sulfuric Acid and obtains ammonium sulfate.Said process respectively obtains sodium acetate, first
Alcohol, diazonium Organic substance and ammonium sulfate, after separation, the COD of water is less than 1000PPM, can enter industrial wastewater treatment system；This
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 substance, methanol and water mixed solution, sodium and ammonium acetate salt weight
Amount percentage composition about 21.5～23.0%, diazonium Organic substance about 2.0～2.5%, methanol 15.0～16.0%.
In described step (1), the temperature at the bottom of the tower top of successive reaction side line rectifying column and tower be 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 the
41 blocks of plates, 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), alkali liquor preferred 50wt%NaOH solution, material liquid with the mass ratio of 50%NaOH alkali liquor is
1∶0.146。
In described step (1), tail gas ammonia uses sulfuric acid treatment to obtain ammonium sulfate.
In described step (2) multiple stage of countercurrent liquid-liquid extraction method, described extractant is industry hexamethylene.Extractant with contain
Sodium acetate, diazonium Organic substance and aqueous mixtures feed weight ratio be: 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,
Operation temperature is 10.5～29.5 DEG C.
In described step (3), flash column operation pressure is 0.10～0.15*105Temperature at the bottom of Pa, tower top and tower is respectively
It it is 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
3 blocks of plates.
The continuous external circulation reaction side line rectification of the present invention and liquid-liquid extraction combination process sodium and ammonium acetate salt, diazonium Organic substance,
Methanol and the method for water mixed solution, concrete grammar is as follows: ammonium and sodium acetate, diazonium Organic substance, methanol and water mixing are molten
Liquid adds in mixing channel with 50%NaOH in 1: 0.146 ratio, is added by reaction side line rectifying column middle and lower part charging aperture after mixing
In reaction side line rectifying column, tower bottoms, by circulating pump outer circulation to recycle feed mouth, controls reaction side line rectifying tower top, end temperature
Degree is respectively 41.4～43.1 DEG C and 100.2～102.7 DEG C, and the ammonium salt in material liquid is converted into sodium by reacted side line rectification
Salt, reaction side line rectifying tower top ammonia is absorbed by Waste Sulfuric Acid in absorption cell, and forms ammonium sulfate, and lateral line discharging is more than 95%
Methanol, reaction side line rectifier bottoms discharging is to liquid reducing chamber；In liquid reducing chamber, the diazonium organic wastewater containing sodium acetate is multistage inverse
Flow liquid liquid extraction tower middle and upper part enter, extractant normal hexane the middle and lower part of multiple stage of countercurrent liquid-liquid extraction tower add, extractant with
Liquid-liquid extraction tower charge ratio is 0.4～1.2: 1；After multiple stage of countercurrent liquid-liquid extraction, liquid-liquid extraction top of tower discharging is containing diazonium
Organic normal hexane, enters flash column containing the organic normal hexane of diazonium, and operation pressure is 0.10～0.15*105Pa, 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, process through flash column, respectively obtain content >=97%
Diazonium Organic substance and normal hexane, n-hexane recycle to liquid-liquid extraction tower, multiple stage of countercurrent liquid-liquid extraction tower bottom discharging is containing acetic acid
The aqueous solution of sodium, processes through evaporation and drying unit, respectively obtains 98% sodium acetate and industry water, and in industry water, COD is less than
1000PPM, industry water recycles as water for industrial use.
The present invention uses the technique that successive reaction side line rectification and multiple stage of countercurrent liquid-liquid extraction combine, process sodium and ammonium acetate salt,
Diazonium Organic substance, methanol and water mixed solution, through primary first-order equation side line rectification, can be converted into sodium salt by ammonium salt therein, and
Isolate tail gas ammonia and methanol, obtain containing sodium acetate, diazonium Organic substance and aqueous mixtures, then it is organic to contain sodium acetate, diazonium
Thing and aqueous mixtures carry out multiple stage of countercurrent liquid-liquid extraction, respectively obtain sodium acetate aqueous solution and diazonium Organic substance, extractant mixing
Thing, sodium acetate aqueous solution obtains fine chemicals sodium acetate through evaporation process, and diazonium Organic substance, extractant mixture flash distillation divide
From, diazonium content of organics >=97%, the extractant that multiple stage of countercurrent liquid-liquid extraction is used is normal hexane, can recycle.
Respectively obtaining more than 95% methanol and tail gas ammonia in reaction side line distillation process, 95% methanol recycles as solvent, tail simultaneously
Gas ammonia processes through Waste Sulfuric Acid and obtains ammonium sulfate.Use the inventive method, above-mentioned processing procedure respectively obtain sodium acetate, methanol,
Diazonium Organic substance and ammonium sulfate, after separation, the COD of water is less 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 with detailed description of the invention
It is limited, but is defined in the claims.
Accompanying drawing explanation
Fig. 1 is that continuous external circulation reacts side line rectification and liquid-liquid extraction combination processes sodium and ammonium acetate salt-diazonium nitrogen organic-first
The schematic flow sheet of alcohol-water mixed solution.
Detailed description of the invention
Below by specific embodiment, technical solutions according to the invention are further described in detail, but it is necessary to note that
Following example are served only for the description to summary of the invention, are not intended that limiting the scope of the invention.
The continuous external circulation reaction side line rectification of the present invention and liquid-liquid extraction combination process sodium and ammonium acetate salt-diazonium nitrogen organic-
The method of methanol-water mixed solution, reaction side line rectification and multiple stage of countercurrent liquid-liquid extraction coupling apparatus and technological process reference Fig. 1,
Wherein 1 is dashpot, and 2 is liquid reducing chamber, and 3 is reaction side line rectification tower reactor, and 4 is charging aperture, and 5 is reaction side line rectifying column,
6 is recycle feed mouth, and 7 is side line discharge, and 8 is absorption cell, and 9 is circulating pump, and 10 is multiple stage of countercurrent liquid-liquid extraction tower,
11 is raw material, and 12 is 50%NaOH solution, and 13 is raw material and 50%NaOH solution mixed feeding, and 14 is reaction side line essence
Evaporating column overhead discharging, 15 is Waste Sulfuric Acid, and 16 is lateral line discharging, and 17 is tower bottoms recycle feed, and 18 is multi-stage countercurrent liquid liquid
Extraction tower feeds, and 19 is multiple stage of countercurrent liquid-liquid extraction top of tower discharging, and 20 is the extractant of multiple stage of countercurrent liquid-liquid extraction tower, and 21
For multiple stage of countercurrent liquid-liquid extraction tower bottom discharging, 22 is flash column, and 23 is flash column bottom discharge, and 24 go out for flash column top
Material, 25 is evaporation and drying unit, and 26 is evaporation and drying unit bottom discharge, and 27 is evaporation and drying unit top discharge.
Using sodium that certain company provides and ammonium acetate salt, diazonium Organic substance, methanol and water mixed solution is raw material, reacts side line
The operation of rectifying column is carried out at ambient pressure, and tower internal diameter is 25mm, built-in φ 3*3 θ type stainless steel helices, through by standards system
Measuring, this height equivalent to one theoretical plate HETP=27mm, tower reactor coiled electrical heating, raw material, liquid-liquid extraction agent feed and respectively fill
Putting discharging etc. all to measure with glass rotameter, reaction side line rectifying column uses exteenal reflux.
Ammonium and sodium acetate, diazonium Organic substance, methanol and water mixed solution 11 compare by 1: 0.146 with 50%NaOH solution 12
Example adds mixing channel 1, is added in reaction side line rectifying column 5 by reaction side line rectifying column 5 middle and lower part charging aperture 4, tower after mixing
In still 3, solution is recycled to recycle feed mouth 6 by circulating pump 9, controls reaction side line rectifying column 5 tower top, end temperature respectively
41.4～43.1 DEG C and 100.2～102.7 DEG C, control tower fight back flow 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% methanol, from reaction side line essence
Evaporating side line discharge 7 extraction of tower 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 enters
Material 18, from diazonium organic wastewater containing sodium acetate in liquid reducing chamber 2, enters in multiple stage of countercurrent liquid-liquid extraction tower 10 middle and upper part,
Extractant normal hexane 20 adds in multiple stage of countercurrent liquid-liquid extraction tower 10 middle and lower part, extractant and the diazonium Organic substance containing sodium acetate
Wastewater feed ratio is 1: 1, and after liquid-liquid extraction, extraction tower 10 top discharge 19 is containing the organic normal hexane of diazonium, containing diazonium
Organic normal hexane processes through flash column 22, and flash column bottom discharge 23 and top discharge 24 respectively obtain diazonium Organic substance
And normal hexane, normal hexane i.e. top discharge 24 is recycled 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, processes through evaporation and drying unit 25, and bottom discharge 26 and top discharge 27 respectively obtain
98% sodium acetate and industry water, in industry water, COD is less than 1000PPM, and industry water can recycle as water for industrial use.
Described reaction side line rectification and the preferred process conditions of liquid-liquid extraction separation process are as follows:
Top, end temperature, reflux ratio, the feed entrance points such as reaction side line rectifying column 5, multistage liquid-liquid extraction tower 10 and flash column 22
And the number of plates is shown in Table 1.
Table 1 reacts side line rectification and liquid-liquid extraction separation process conditions
Analyzing through HP chromatograph, continuous external circulation reaction side line rectification and liquid-liquid extraction combination process sodium and ammonium acetate salt-diazonium
The results are shown in Table shown in 2 of nitrogen organic-methanol-water mixed solution.
The reaction side line rectification of table 2 continuous external circulation and liquid-liquid extraction combination process sodium and ammonium acetate salt-diazonium nitrogen organic-methanol-
The result of water mixed solution
Table 2 (Continued)
Claims (8)
1. a continuous external circulation reaction side line rectification and liquid-liquid extraction combination process sodium and ammonium acetate salt, diazonium Organic substance, first
The method of alcohol and water mixed solution, comprises the following steps:
1) from reaction after raw material sodium and ammonium acetate salt, diazonium Organic substance, methanol and water mixed solution are mixed by reaction ratio with alkali liquor
Side line rectifying column middle and lower part material inlet adds, and reaction side line tower bottom of rectifying tower liquid is by outer circulation pump pump to material inlet
The recycle feed mouth of side carries out outer circulation, reacted side line rectification, and the ammonium salt in material liquid is converted into sodium salt, reacts side line
Rectification bottom discharge is to liquid reducing chamber, and liquid reducing chamber discharging is containing sodium acetate, diazonium Organic substance and aqueous mixtures, reacts side line rectification
Tower side line, tower top respectively obtain more than 95wt% methanol and tail gas ammonia；
2) multistage liquid-liquid extraction tower is entered containing sodium acetate, diazonium Organic substance and aqueous mixtures, with hexamethylene as extractant, through many
Stage countercurrent liquid-liquid extraction, at the bottom of tower, tower top respectively obtain sodium acetate aqueous solution and comprise the organic facies of diazonium Organic substance, extractant,
Obtaining 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 of generation contains
Amount is less than 0.1wt%；
3) multistage liquid-liquid extraction tower top is the organic facies being mainly made up of extractant and diazonium Organic substance, processes through flash column, tower
Top is extracted agent, is recycled to multistage liquid liquid counter-current extraction tower and recycles, obtains content >=97wt% diazonium Organic substance at the bottom of tower.
Continuous external circulation the most according to claim 1 reaction side line rectification and liquid-liquid extraction combination process sodium and ammonium acetate salt,
The method of diazonium Organic substance, methanol and water mixed solution, it is characterised in that: described sodium and ammonium acetate salt, diazonium Organic substance,
In methanol and water mixed solution, weight percentage is sodium and ammonium acetate salt 21.5～23.0%, diazonium Organic substance 2.0～2.5%,
Methanol 15.0～16.0%.
Continuous external circulation the most according to claim 1 and 2 reaction side line rectification and liquid-liquid extraction combination process sodium and ammonium vinegar
Hydrochlorate, diazonium Organic substance, methanol and the method for water mixed solution, it is characterised in that: in described step (1), the most instead
The temperature at the bottom of the tower top of side line rectifying column and tower is answered to be respectively 41.4～43.1 DEG C and 100.2～102.7 DEG C.
Continuous external circulation the most according to claim 1 and 2 reaction side line rectification and liquid-liquid extraction combination process sodium and ammonium vinegar
Hydrochlorate, diazonium Organic substance, methanol and the method for water mixed solution, it is characterised in that: in described step (1), react side
The number of theoretical plate of line rectifying column is 47, and material inlet position, is followed at the 13rd block of plate in the 41st block of plate, lateral line discharging position
Ring gating location is at the 36th block of plate.
Continuous external circulation the most according to claim 1 and 2 reaction side line rectification and liquid-liquid extraction combination process sodium and ammonium vinegar
Hydrochlorate, diazonium Organic substance, methanol and the method for water mixed solution, it is characterised in that: in described step (1), alkali liquor is
50wt%NaOH solution, material liquid is 1: 0.146 with the mass ratio of 50wt%NaOH alkali liquor.
Continuous external circulation the most according to claim 1 and 2 reaction side line rectification and liquid-liquid extraction combination process sodium and ammonium vinegar
Hydrochlorate, diazonium Organic substance, methanol and the method for water mixed solution, it is characterised in that: in described step (2), extractant
With containing sodium acetate, diazonium Organic substance and aqueous mixtures feed weight ratio it is: 0.4～1.2: 1.
Continuous external circulation the most according to claim 1 and 2 reaction side line rectification and liquid-liquid extraction combination process sodium and ammonium vinegar
Hydrochlorate, diazonium Organic substance, methanol and the method for water mixed solution, it is characterised in that: described step (2) multi-stage countercurrent liquid
In liquid-liquid extraction method, multiple stage of countercurrent liquid-liquid extraction tower number of theoretical plate is 4, and operation temperature is 10.5～29.5 DEG C.
Continuous external circulation the most according to claim 1 and 2 reaction side line rectification and liquid-liquid extraction combination process sodium and ammonium vinegar
Hydrochlorate, diazonium Organic substance, methanol and the method for water mixed solution, it is characterised in that: in described step (3), flash column
Operation pressure is 0.10～0.15*105Temperature at the bottom of Pa, tower top and tower is 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.
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| 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 |
| 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 |
| CN112499868B (en) * | 2020-11-30 | 2023-04-18 | 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 |
| 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 |
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