CN109180442A - A kind of method that the adsorbing coupled technique of extracting rectifying-recycles methyl tertiary butyl ether(MTBE) in pharmacy procedure waste liquid - Google Patents
A kind of method that the adsorbing coupled technique of extracting rectifying-recycles methyl tertiary butyl ether(MTBE) in pharmacy procedure waste liquid Download PDFInfo
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- CN109180442A CN109180442A CN201811270411.7A CN201811270411A CN109180442A CN 109180442 A CN109180442 A CN 109180442A CN 201811270411 A CN201811270411 A CN 201811270411A CN 109180442 A CN109180442 A CN 109180442A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/36—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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Abstract
The invention belongs to solvent recovery fields, and in particular to a kind of method that the adsorbing coupled technique of extracting rectifying-recycles methyl tertiary butyl ether(MTBE) in pharmacy procedure waste liquid.Extractive distillation column is respectively enterd by certain solvent ratio with pharmacy procedure waste liquid using water as extractant, it isolates in extracting rectifying column overhead containing normal butane and methyl tertiary butyl ether(MTBE) crude product, the material of tower reactor enters extractant recovery tower and carries out extractant recycling, and the extractant of tower reactor recycling returns to extractive distillation column recycling after cooling；For the material of extracting rectifying column overhead after phase-splitter is layered, lower layer's water phase is back to extractive distillation column, and upper oil phase enters adsorption dewatering system, obtain the methyl tertiary butyl ether(MTBE) material containing normal butane, into normal butane knockout tower, tower reactor obtains methyl tertiary butyl ether(MTBE), recyclable to use as pharmacy solvent.The present invention existing component water using in waste liquid efficiently avoids the recycling for introducing other components influence methyl tertiary butyl ether(MTBE) as extractant, is a kind of energy-efficient separating technology.
Description
Technical field
The invention belongs to solvent recovery fields, and in particular to a kind of adsorbing coupled technique recycling pharmacy procedure of extracting rectifying-
The method of methyl tertiary butyl ether(MTBE) in waste liquid.
Background technique
4- chloro- 2- (trifluoroacetyl group) anilinechloride hydrate, abbreviation E2, molecular formula: C8H5ClF3NO·HCl·
H2O, molecular weight: 278, No. CAS: 173676-59-0, it is a kind of white or light yellow crystalline powder, main application: as pass
Key intermediate is used for synthesizing anti-AIDS pharmaceutical efavirenz.Intermediate E 2 is using parachloroanilinum as starting material, with pivaloyl
Chlorine first carries out condensation reaction, then through acylation reaction and hydrolysis, most afterwards through being refining to obtain.In condensation reaction and acylation reaction mistake
It needs to carry out in a large amount of methyl tert-butyl ether solvent in journey, reaction process is simultaneously with normal butane, water, ethyl alcohol and the tert-butyl alcohol
Deng generation, after reaction terminates, need first distill solvent, the solvent composition steamed are as follows: 7 ~ 9wt% normal butane, 1 ~ 3wt%
Water, 1.5 ~ 3wt% ethyl alcohol, 0.5 ~ 2wt% tert-butyl alcohol, 83 ~ 90wt% methyl tertiary butyl ether(MTBE).Above-mentioned mixed solvent need to be separated,
The content of methyl tertiary butyl ether(MTBE) is set to be greater than 99.5wt%, moisture is less than 200ppm, and alcohol content is less than 500ppm, makes to reach circulation
With requiring.
For the waste liquid of above-mentioned generation, the recycling of solvent methyl t-butyl ether is a very difficult problem, this be by
There is multiple groups binary azeotropic under normal pressure in the system, ethanol content is in the binary azeotropic composition of ethyl alcohol and methyl tertiary butyl ether(MTBE)
7.7wt%, azeotropic temperature are 57.9 DEG C；Ethanol content is 95.6wt% in the binary azeotropic of ethyl alcohol and water composition, and azeotropic temperature is
78.2℃；T butanol content is 87.5wt% in the binary azeotropic of the tert-butyl alcohol and water composition, and azeotropic temperature is 80.3 DEG C；Methyl- tert
Methyl tertbutyl ether content is 94.1wt% in the binary azeotropic of butyl ether and water composition, and azeotropic temperature is 55.9 DEG C；Normal butane with
Normal butane content is 98.7wt% in the binary azeotropic composition of water, and azeotropic temperature is -1.72 DEG C, therefore is difficult to by conventional distillation
Water, ethyl alcohol and the tert-butyl alcohol in mixture are removed, is needed through special extract rectification, such as extracting rectifying or azeotropic distillation, but is passed through
Extracting rectifying or azeotropic distillation need to introduce third component as extractant or entrainer, and methyl tertiary butyl ether(MTBE) is caused to make in circulation
Used time unavoidably introduces other impurities, and then influences the quality of intermediate E 2.
Summary of the invention
It is an object of the present invention to provide methyl- tert fourths in a kind of adsorbing coupled technique recycling pharmacy procedure waste liquid of extracting rectifying-
The method of base ether, in selective system existing component water as extractant, by separation of extractive distillation go out ethyl alcohol in solvent and
The tert-butyl alcohol makes alcohol content be less than 500ppm, sieves adsorption dewatering by many-level molecule, so that the water content of solvent is less than 200ppm, most
By compression rectification, solvent methyl t-butyl ether content is made to be greater than 99.5wt%, realizes that solvent is recycled, this method is effectively
It solves the problems, such as the recycling difficulty of solvent methyl t-butyl ether in production process, and reduces the consumption of raw material, improve anti-
The economic benefit of AIDS-treating medicine efavirenz key intermediate production process.
In order to solve the above-mentioned technical problem, the present invention is realized using following following technical solution:
A kind of method that the adsorbing coupled technique of extracting rectifying-recycles methyl tertiary butyl ether(MTBE) in pharmacy procedure waste liquid, including following step
It is rapid:
Step S1: using water as extractant, with the pharmacy containing methyl tertiary butyl ether(MTBE), normal butane, ethyl alcohol, the tert-butyl alcohol and a small amount of water
Process waste, than entering in tower from the upper feed inlet of extractive distillation column and lower part feed inlet respectively, is extracting essence by certain solvent
It evaporates column overhead and obtains the methyl tertiary butyl ether(MTBE) crude product containing normal butane and a small amount of water, wherein the total content of ethyl alcohol and the tert-butyl alcohol is less than
500ppm, tower reactor obtain the extraction agent solution containing ethyl alcohol, the tert-butyl alcohol；
Step S2: the material of extractive distillation column tower reactor enters in tower from the middle part of extractant recovery tower, carries out extractant recycling, tower
Ethyl alcohol, tert-butyl alcohol mixed liquor containing a small amount of water are isolated in top, and the extractant of tower reactor recycling returns to extractive distillation column after cooling and follows
Ring uses；
Step S3: for the material of extracting rectifying column overhead after phase-splitter is layered, bottom aqueous amount is that the water phase of 99wt% is back to extraction
Rectifying column is taken, the oil on upper layer is mutually mainly the mixture of methyl tertiary butyl ether(MTBE) and normal butane, and water content is less than 2wt%, alcohol content
Less than 500ppm, the methyl tertiary butyl ether(MTBE) containing normal butane is obtained through level Four adsorption dewatering into four concatenated adsorption dewatering towers
Material, water content are less than 200ppm, and alcohol content is less than 500ppm；
Step S4: the material that adsorption dewatering tower comes out enters in tower from the middle part of normal butane knockout tower, carries out compression rectification, tower top
The normal butane that content is greater than 99.5% is isolated, tower reactor obtains the methyl tertiary butyl ether(MTBE) that content is greater than 99.5%, is recycled as system
Medicine solvent uses.
Further, the operating condition of the extractive distillation column are as follows: tower internals type is column plate or filler, and number of theoretical plate is
28 ~ 36, operating pressure is 100 ~ 110kPa, and overhead reflux ratio is 1.6 ~ 4.5, the feed volume of extractant and pharmacy procedure waste liquid
Than being 0.2 ~ 0.9, tower top temperature is 49 ~ 54 DEG C, and bottom temperature is 64 ~ 69 DEG C.
Further, the operating condition of the extractant recovery tower are as follows: tower internals type is column plate or filler, number of theoretical plate
Be 18 ~ 26, operating pressure be 100 ~ 110kPa, overhead reflux ratio be 3 ~ 7, tower top temperature be 75 ~ 80 DEG C, bottom temperature be 100 ~
105℃。
Further, the operating condition of the adsorption dewatering tower: adsorption dewatering tower is tubular heat exchanger, and tube side, which is equipped with, to be divided
Son sieve, adsorption operations pressure are 100 ~ 200kPa, and adsorption temp is 25 ~ 55 DEG C.
Further, the operating condition of the normal butane knockout tower are as follows: tower internals type is column plate or filler, number of theoretical plate
It is 26 ~ 38, operating pressure is 400 ~ 600kPa, and overhead reflux ratio is 2.5 ~ 5.4, and tower top temperature is 42 ~ 57 DEG C, and bottom temperature is
107~124℃。
Remarkable advantage of the invention is:
(1) existing component water in waste liquid is selected to effectively realize as extractant using the adsorbing coupled technique of extracting rectifying-
The separation of methyl tertiary butyl ether(MTBE) and ethyl alcohol, the tert-butyl alcohol, water, solves the system since there are multiple groups binary azeotropics in waste liquid
Problem is separated, and avoids the recycling for introducing other components influence methyl tertiary butyl ether(MTBE).
(2) using the method for methyl tertiary butyl ether(MTBE) in the adsorbing coupled technique recycling pharmacy procedure waste liquid of extracting rectifying-, have
Energy consumption, the discharge amount of equipment investment and waste water for reducing to effect separation carry out interrupted extraction removing with conventionally employed a large amount of water
The technique of alcohol is compared, and the adsorbing coupled technique of extracting rectifying-can save energy consumption 30-45%, saves equipment investment 18-32%, waste water row
High-volume reduce 80%；
(3) method of the invention is used, the methyl tertiary butyl ether(MTBE) purity of recycling is greater than 99.5%, and moisture is less than 200ppm, and alcohol contains
Amount is less than 500ppm.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the embodiment of the present invention.
In figure: T1 is extractive distillation column；T2 is extractant recovery tower；T3 is positive butane splitter；V1 is phase-splitter；A1~
A4 is adsorption dewatering tower；E1 is feed preheater；E2 is extractive distillation column condenser；E3 is extracting rectifying tower reboiler；E4 is
Extractant recovery tower condenser；E5 is that extractant recycles tower reboiler；E6 is positive butane splitter condenser；E7 is normal butane point
From tower reboiler.PL1 is pharmacy procedure waste liquid feed pipe, and PL2 is that pharmacy procedure waste liquid preheats laggard expects pipe, and PL3 is methyl- tert
Butyl ether crude product discharge nozzle, PL4 are phase-splitter oil phase discharge nozzle, and PL5 is adsorption dewatering tower discharge nozzle, and PL6 is phase-splitter oil phase
Discharge nozzle, PL7 are extractive distillation column tower reactor discharge nozzle, and PL8 is that extractant recycles column overhead discharge nozzle, and PL9 is extractant recycling
Tower tower reactor discharge nozzle, PL10 are extractant circulation pipe, and PL11 is extractive distillation column extractant feed pipe, and PL12 is normal butane separation
Column overhead discharge nozzle, PL13 are positive butane splitter tower reactor discharge nozzle.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings and embodiments.
As shown in Figure 1, present embodiments providing first in a kind of adsorbing coupled technique recycling pharmacy procedure waste liquid of extracting rectifying-
The method of base tertbutyl ether, comprising the following steps:
Step S1: using water as extractant, with the pharmacy containing methyl tertiary butyl ether(MTBE), normal butane, ethyl alcohol, the tert-butyl alcohol and a small amount of water
Process waste, than entering in tower from the upper feed inlet of extractive distillation column and lower part feed inlet respectively, is extracting essence by certain solvent
It evaporates column overhead and obtains the methyl tertiary butyl ether(MTBE) crude product containing normal butane and a small amount of water, wherein the total content of ethyl alcohol and the tert-butyl alcohol is less than
500ppm, tower reactor obtain the extraction agent solution containing ethyl alcohol, the tert-butyl alcohol；
Step S2: the material of extractive distillation column tower reactor enters in tower from the middle part of extractant recovery tower, carries out extractant recycling, tower
Ethyl alcohol, tert-butyl alcohol mixed liquor containing a small amount of water are isolated in top, and the extractant of tower reactor recycling returns to extractive distillation column after cooling and follows
Ring uses；
Step S3: for the material of extracting rectifying column overhead after phase-splitter is layered, bottom aqueous amount is that the water phase of 99wt% is back to extraction
Rectifying column is taken, the oil on upper layer is mutually mainly the mixture of methyl tertiary butyl ether(MTBE) and normal butane, and water content is less than 2wt%, alcohol content
Less than 500ppm, the methyl tertiary butyl ether(MTBE) containing normal butane is obtained through level Four adsorption dewatering into four concatenated adsorption dewatering towers
Material, water content are less than 200ppm, and alcohol content is less than 500ppm；
Step S4: the material that adsorption dewatering tower comes out enters in tower from the middle part of normal butane knockout tower, carries out compression rectification, tower top
The normal butane that content is greater than 99.5% is isolated, tower reactor obtains the methyl tertiary butyl ether(MTBE) that content is greater than 99.5%, is recycled as system
Medicine solvent uses.
In the present embodiment, the operating condition of the extractive distillation column T1 are as follows: tower internals type is column plate or filler, theory
Plate number is 28 ~ 36, and operating pressure is 100 ~ 110kPa, and overhead reflux ratio is 1.6 ~ 4.5, extractant and pharmacy procedure waste liquid into
Expect that volume ratio is 0.2 ~ 0.9, tower top temperature is 49 ~ 54 DEG C, and bottom temperature is 64 ~ 69 DEG C.
In the present embodiment, the operating condition of the extractant recovery tower T2 are as follows: tower internals type is column plate or filler, reason
It is 18 ~ 26 by plate number, operating pressure is 100 ~ 110kPa, and overhead reflux ratio is 3 ~ 7, and tower top temperature is 75 ~ 80 DEG C, bottom temperature
It is 100 ~ 105 DEG C.
In the present embodiment, the operating condition of the adsorption dewatering tower A1 ~ A4: adsorption dewatering tower is tubular heat exchanger,
Tube side is equipped with molecular sieve, and adsorption operations pressure is 100 ~ 200kPa, and adsorption temp is 25 ~ 55 DEG C.
In the present embodiment, the operating condition of the normal butane knockout tower T3 are as follows: tower internals type is column plate or filler, reason
It is 26 ~ 38 by plate number, operating pressure is 400 ~ 600kPa, and overhead reflux ratio is 2.5 ~ 5.4, and tower top temperature is 42 ~ 57 DEG C, tower reactor
Temperature is 107 ~ 124 DEG C.
The following are two specific examples of the present embodiment.
Embodiment 1:
Using process flow shown in FIG. 1, extractive distillation column T1 tower body material is SUS304, and the filling regular silk screen of BX is filled out in tower
Material, tower diameter 1200mm, number of theoretical plate 32, extractant feeds from the 6th piece of theoretical plate, and pharmacy procedure waste liquid is from the 21st piece of theory
Plate charging.Extractant recovery tower T2 tower body material is SUS304, and the regular wire packing of BX is filled in tower, and tower diameter 500mm is theoretical
Plate number is the 24, the 14th piece of theoretical plate charging.Normal butane knockout tower T3 tower body material is SUS304, and the filling regular silk screen of BX is filled out in tower
Material, tower diameter 600mm, number of theoretical plate 30, the 13rd piece of theoretical plate charging.Adsorption dewatering tower A1 ~ A4 tower body material is SUS304,
Tower diameter is 1200mm, is highly 3000mm, and the tubulation of 503 DN38 is equipped in tower, and 13X type molecular sieve is filled in tubulation.
The feed rate of pharmacy procedure waste liquid is 2500kg/h, is entered from feed inlet under extractive distillation column T1, feeding temperature
32 DEG C, feed composition: normal butane 8%, water 1.5%, ethyl alcohol 2%, the tert-butyl alcohol 2%, methyl tertiary butyl ether(MTBE) 86.5%；The charging of extractant water
Amount is 800kg/h, is entered from the enterprising material mouth of extractive distillation column T1.The operating condition of extractive distillation column T1: operating pressure is
101kPa, 52.2 DEG C of tower top temperature, 64.7 DEG C of column bottom temperature, reflux ratio 2.5.Extractant recovery tower T2 operating condition: operation pressure
Power 101kPa, 77.5 DEG C of tower top temperature, 102.2 DEG C of column bottom temperature, reflux ratio 5.Normal butane knockout tower T3 operating condition: operation pressure
Power 400kPa, 42 DEG C of tower top temperature, 107 DEG C of column bottom temperature, reflux ratio 4.Adsorption dewatering tower A1 ~ A4 operating condition: operating pressure
For 101kPa, adsorption temp is 30 DEG C.
Under the above conditions, its purity of methyl tert-butyl ether product of normal butane knockout tower T3 tower reactor recycling is 99.6%, water
It is divided into 165ppm, ethanol content 146ppm, tert-butyl alcohol alcohol content is 125ppm, reaches and index can be recycled.
Embodiment 2:
Using process flow shown in FIG. 1, extractive distillation column T1 tower body material is SUS304, and the filling regular silk screen of BX is filled out in tower
Material, tower diameter 1200mm, number of theoretical plate 32, extractant feeds from the 6th piece of theoretical plate, and pharmacy procedure waste liquid is from the 21st piece of theory
Plate charging.Extractant recovery tower T2 tower body material is SUS304, and the regular wire packing of BX is filled in tower, and tower diameter 500mm is theoretical
Plate number is the 24, the 14th piece of theoretical plate charging.Normal butane knockout tower T3 tower body material is SUS304, and the filling regular silk screen of BX is filled out in tower
Material, tower diameter 600mm, number of theoretical plate 30, the 13rd piece of theoretical plate charging.Adsorption dewatering tower A1 ~ A4 tower body material is SUS304,
Tower diameter is 1200mm, is highly 3000mm, and the tubulation of 503 DN38 is equipped in tower, and 13X type molecular sieve is filled in tubulation.
The feed rate of pharmacy procedure waste liquid is 2000kg/h, is entered from feed inlet under extractive distillation column T1, feeding temperature
32 DEG C, feed composition: normal butane 7%, water 2%, ethyl alcohol 2.5%, the tert-butyl alcohol 1.5%, methyl tertiary butyl ether(MTBE) 87%；The charging of extractant water
Amount is 1000kg/h, is entered from the enterprising material mouth of extractive distillation column T1.The operating condition of extractive distillation column T1: operating pressure is
110kPa, 54 DEG C of tower top temperature, 69 DEG C of column bottom temperature, reflux ratio 2.Extractant recovery tower T2 operating condition: operating pressure
110kPa, 79.2 DEG C of tower top temperature, 104.8 DEG C of column bottom temperature, reflux ratio 3.5.Normal butane knockout tower T3 operating condition: operation pressure
Power 600kPa, 57 DEG C of tower top temperature, 124 DEG C of column bottom temperature, reflux ratio 2.5.Adsorption dewatering tower A1 ~ A4 operating condition: operation pressure
Power is 110kPa, and adsorption temp is 32 DEG C.
Under the above conditions, its purity of methyl tert-butyl ether product of normal butane knockout tower T3 tower reactor recycling is 99.8%, water
It is divided into 142ppm, ethanol content 123ppm, tert-butyl alcohol alcohol content is 102ppm, reaches and index can be recycled.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (6)
1. the method for methyl tertiary butyl ether(MTBE), feature exist in a kind of adsorbing coupled technique recycling pharmacy procedure waste liquid of extracting rectifying-
In: extractive distillation column is respectively enterd by certain solvent ratio with pharmacy procedure waste liquid using water as extractant, in extractive distillation column tower
Top is isolated containing normal butane and methyl tertiary butyl ether(MTBE) crude product, and the material of tower reactor enters extractant recovery tower and carries out extractant recycling,
The extractant of tower reactor recycling returns to extractive distillation column recycling after cooling；The material of extracting rectifying column overhead is through phase-splitter point
After layer, lower layer's water phase is back to extractive distillation column, and upper oil phase enters adsorption dewatering system, obtains the methyl- tert fourth containing normal butane
Base ether material, into normal butane knockout tower, tower reactor obtains methyl tertiary butyl ether(MTBE), recyclable to use as pharmacy solvent.
2. methyl- tert fourth in the adsorbing coupled technique recycling pharmacy procedure waste liquid of a kind of extracting rectifying-according to claim 1
The method of base ether, it is characterised in that: specifically includes the following steps:
Step S1: using water as extractant, with the pharmacy containing methyl tertiary butyl ether(MTBE), normal butane, ethyl alcohol, the tert-butyl alcohol and a small amount of water
Process waste, than entering in tower from the upper feed inlet of extractive distillation column and lower part feed inlet respectively, is extracting essence by certain solvent
It evaporates column overhead and obtains the methyl tertiary butyl ether(MTBE) crude product containing normal butane and a small amount of water, wherein the total content of ethyl alcohol and the tert-butyl alcohol is less than
500ppm, tower reactor obtain the extraction agent solution containing ethyl alcohol, the tert-butyl alcohol；
Step S2: the material of extractive distillation column tower reactor enters in tower from the middle part of extractant recovery tower, carries out extractant recycling, tower
Ethyl alcohol, tert-butyl alcohol mixed liquor containing a small amount of water are isolated in top, and the extractant of tower reactor recycling returns to extractive distillation column after cooling and follows
Ring uses；
Step S3: for the material of extracting rectifying column overhead after phase-splitter is layered, bottom aqueous amount is that the water phase of 99wt% is back to extraction
Rectifying column is taken, the oil on upper layer is mutually mainly the mixture of methyl tertiary butyl ether(MTBE) and normal butane, and water content is less than 2wt%, alcohol content
Less than 500ppm, the methyl tertiary butyl ether(MTBE) containing normal butane is obtained through level Four adsorption dewatering into four concatenated adsorption dewatering towers
Material, water content are less than 200ppm, and alcohol content is less than 500ppm；
Step S4: the material that adsorption dewatering tower comes out enters in tower from the middle part of normal butane knockout tower, carries out compression rectification, tower top
The normal butane that content is greater than 99.5% is isolated, tower reactor obtains the methyl tertiary butyl ether(MTBE) that content is greater than 99.5%, is recycled as system
Medicine solvent uses.
3. methyl- tert fourth in the adsorbing coupled technique recycling pharmacy procedure waste liquid of a kind of extracting rectifying-according to claim 1
The method of base ether, it is characterised in that: the operating condition of the extractive distillation column are as follows: tower internals type is column plate or filler, theory
Plate number is 28 ~ 36, and operating pressure is 100 ~ 110kPa, and overhead reflux ratio is 1.6 ~ 4.5, extractant and pharmacy procedure waste liquid into
Expect that volume ratio is 0.2 ~ 0.9, tower top temperature is 49 ~ 54 DEG C, and bottom temperature is 64 ~ 69 DEG C.
4. methyl- tert fourth in the adsorbing coupled technique recycling pharmacy procedure waste liquid of a kind of extracting rectifying-according to claim 1
The method of base ether, it is characterised in that: the operating condition of the extractant recovery tower are as follows: tower internals type is column plate or filler, reason
It is 18 ~ 26 by plate number, operating pressure is 100 ~ 110kPa, and overhead reflux ratio is 3 ~ 7, and tower top temperature is 75 ~ 80 DEG C, bottom temperature
It is 100 ~ 105 DEG C.
5. methyl- tert fourth in the adsorbing coupled technique recycling pharmacy procedure waste liquid of a kind of extracting rectifying-according to claim 1
The method of base ether, it is characterised in that: the operating condition of the adsorption dewatering tower: adsorption dewatering tower is tubular heat exchanger, tube side
Equipped with molecular sieve, adsorption operations pressure is 100 ~ 200kPa, and adsorption temp is 25 ~ 55 DEG C.
6. methyl- tert fourth in the adsorbing coupled technique recycling pharmacy procedure waste liquid of a kind of extracting rectifying-according to claim 1
The method of base ether, it is characterised in that: the operating condition of the normal butane knockout tower are as follows: tower internals type is column plate or filler, reason
It is 26 ~ 38 by plate number, operating pressure is 400 ~ 600kPa, and overhead reflux ratio is 2.5 ~ 5.4, and tower top temperature is 42 ~ 57 DEG C, tower reactor
Temperature is 107 ~ 124 DEG C.
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| CN110501200A (en) * | 2019-09-23 | 2019-11-26 | 吉林师范大学 | A kind of black nightshade effective ingredient that can be recycled is extracted and separation method |
| CN113842852A (en) * | 2021-10-29 | 2021-12-28 | 聊城鲁西甲胺化工有限公司 | Process and system for annual production of 20 ten thousand tons of methylamine |
| CN114409496A (en) * | 2021-12-31 | 2022-04-29 | 国家能源集团宁夏煤业有限责任公司 | Method and device for separating 1-octene from Fischer-Tropsch synthetic oil |
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| CN116332713A (en) * | 2022-07-28 | 2023-06-27 | 四川熔增环保科技有限公司 | Method for recycling organic solvent in waste liquid in drug synthesis process |
| CN116332737A (en) * | 2022-07-28 | 2023-06-27 | 四川熔增环保科技有限公司 | Recycling method of methyl tertiary butyl ether waste solvent |
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| CN116332713B (en) * | 2022-07-28 | 2024-03-12 | 四川熔增环保科技有限公司 | Method for recycling organic solvent in waste liquid in drug synthesis process |
| CN116332737B (en) * | 2022-07-28 | 2024-03-12 | 四川熔增环保科技有限公司 | Recycling method of methyl tertiary butyl ether waste solvent |
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