CN108129266A - A kind of process for detaching high-moisture low carbon mixed alcohol - Google Patents
A kind of process for detaching high-moisture low carbon mixed alcohol Download PDFInfo
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- CN108129266A CN108129266A CN201711348455.2A CN201711348455A CN108129266A CN 108129266 A CN108129266 A CN 108129266A CN 201711348455 A CN201711348455 A CN 201711348455A CN 108129266 A CN108129266 A CN 108129266A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
- C07C29/82—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by azeotropic distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention is a kind of process for detaching high-moisture low carbon mixed alcohol, is included the following steps：First, raw material by preheater is preheated, enters in crude tower after preheating and raw material is detached；Mixture is divided into water phase and mixing alcohol phase containing a small amount of alcohol in Phase separation tank；It mixes alcohol phase to return in crude tower, the water phase containing a small amount of alcohol enters in stripper；Split-phase again is carried out in the azeotropic mixture rework solution liquid phase separation tank of butanol, amylalcohol and water；Waste water after qualification is sent into sewage disposal system；Raw material dehydration detaches.The present invention provides a kind of process for detaching high-moisture low carbon mixed alcohol, present invention process is simple, short flow, low energy consumption, reasonable design is combined with Phase separation technology using distillation technology, can effectively deviate from the most of moisture in raw material, subsequently to obtain each monomeric polyol, necessary condition is provided.
Description
Technical field
The present invention relates to technical field of chemical separation more particularly to a kind of technique sides for detaching high-moisture low carbon mixed alcohol
Method.
Background technology
Low carbon mixed alcohol main source is coal liquifaction industry, methanol industry and liquor industry, the component packet of low carbon mixed alcohol
It includes：The higher alcohols such as water, methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, isobutanol, amylalcohol, wherein butanol, penta alcohol and water are deposited
In partial miscibility or insoluble.Water content is all higher in these low carbon mixed alcohols, and usual water content mass ratio is more than 20%, low-carbon
Anhydrous monomeric polyol in mixed alcohol is chemical industry, the very important industrial solvent of pharmaceutical industry and industrial chemicals, however, changing at this stage
The common rectificating method of industrial and commercial bank's industry generally use carries out the abjection of moisture in low carbon mixed alcohol, but is difficult be more than water content
Large quantity of moisture abjection in 20% low carbon mixed alcohol, and the various ingredients in water and low carbon mixed alcohol are there are azeotropic, if
Dehydration problem cannot be effectively solved, follow-up is difficult the monomeric polyol for obtaining high-purity.
Invention content
Present invention seek to address that the deficiencies in the prior art, and a kind of low carbon mixed alcohol for detaching water content and being more than 20% is provided
Process.
The present invention to achieve the above object, using following technical scheme：
A kind of process for detaching high-moisture low carbon mixed alcohol, which is characterized in that include the following steps：
A, first, raw material by preheater is preheated, controls ranging from 85-100 DEG C of preheating temperature, enter after preheating
Raw material is detached in crude tower, controls the reflux ratio ranging from 40-50 of crude tower, tower top pressure 100KPa, tower top temperature
Ranging from 55-60 DEG C of degree, ranging from 125-130 DEG C of bottom temperature；
B, stage casing is substantially water and butanol, amylalcohol component in the tower of crude tower, due to water and butanol and amylalcohol it is insoluble or
Slightly soluble, by crude tower recovered water and butanol, the mixture of amylalcohol, by the mixing alcohol phase with returning to crude tower in heat exchanger one
Heat exchange is cooled to 67 DEG C, then be cooled to 45 DEG C by cooler, is sent into Phase separation tank together, mixture is in Phase separation tank
In be divided into water phase containing a small amount of alcohol and mixing alcohol phase；
C, mixing alcohol phase is returned in crude tower, and the water phase containing a small amount of alcohol is exchanged heat by heat exchanger two to 87 DEG C first, then into
Enter in stripper, control the reflux ratio ranging from 0.5-2, tower top pressure 100KPa, tower top temperature ranging from 82-85 of stripper
DEG C, ranging from 100-101 DEG C of bottom temperature；
D, the azeotropic mixture of butanol, amylalcohol and water is cold through stripper condenser, cooler successively from the overhead extraction of stripper
But to 45 DEG C, split-phase again is carried out in rework solution liquid phase separation tank；
E, the waste water of stripper bottom of towe is again introduced into stripper by stripper reboiler, it is qualified after waste water pass through heat exchange
Device two is sent into sewage disposal system after being cooled to 60 DEG C；
F, the light component in raw material is returned by crude tower condenser in crude tower from the tower top of crude tower, then by rough segmentation
The overhead extraction of tower, tower top side take-off methanol, ethyl alcohol, propyl alcohol and a small amount of aqueous mixtures of crude tower, this part mixes
Methanol product is obtained by rectifying, ethyl alcohol, the third alcohol and water deviate from moisture, then obtain respectively by rectifying by azeotropic essence gold-plating method again
Obtain ethyl alcohol, propyl alcohol product, anhydrous butanol and amylalcohol mixed alcohol pass through rough segmentation tower reboiler from the bottom of towe of crude tower and return to crude tower
In, it is then produced from the bottom of towe of crude tower, subsequently carries out rectified purified obtaining each monomeric polyol.
Particularly, the number of theoretical plate of the crude tower is 80-100 blocks.
The beneficial effects of the invention are as follows：The present invention provides a kind of process for detaching high-moisture low carbon mixed alcohol, this
Invented technology is simple, and short flow, low energy consumption, reasonable design, is combined using distillation technology with Phase separation technology, Neng Gouyou
Most of moisture in the abjection raw material of effect, subsequently to obtain each monomeric polyol, provides necessary condition.
Description of the drawings
Fig. 1 is the process flow chart of the present invention；
In figure：1- preheaters；2- crude tower condensers；3- crude towers；4- rough segmentation tower reboilers；5- heat exchangers one；6- is cold
But device；7- Phase separation tanks；8- heat exchangers two；9- stripper condensers；10- strippers；11- stripper reboilers；
It is described in detail below with reference to the embodiment of the present invention with reference to attached drawing.
Specific embodiment
With reference to embodiment, the invention will be further described：
Embodiment 1
A kind of process for detaching high-moisture low carbon mixed alcohol, includes the following steps：
A, first, raw material is preheated by preheater 1, control preheating temperature is 85 DEG C, and theoretical plate is entered after preheating
Number is detaches raw material in 80 pieces of crude tower 3, and the reflux ratio of control crude tower 3 is 40, tower top pressure 100KPa, tower
It is 55 DEG C to push up temperature, and bottom temperature is 125 DEG C；
B, stage casing is substantially water and butanol, amylalcohol component in the tower of crude tower 3, due to water and butanol and amylalcohol it is insoluble or
Slightly soluble, by 3 recovered water of crude tower and butanol, the mixture of amylalcohol, by the mixing alcohol phase with returning crude tower 3 in heat exchanger 1
Middle heat exchange is cooled to 67 DEG C, then be cooled to 45 DEG C by cooler 6, is sent into Phase separation tank 7 together, and mixture is in liquid liquid point
It is divided into water phase and mixing alcohol phase containing a small amount of alcohol in phase tank 7；
C, mixing alcohol phase is returned in crude tower 3, and the water phase containing a small amount of alcohol is exchanged heat by heat exchanger 28 to 87 DEG C first,
Into in stripper 10, the reflux ratio of control stripper 10 is 0.5, and tower top pressure 100KPa, tower top temperature is 82 DEG C, tower reactor
Temperature is 100 DEG C；
D, the azeotropic mixture of butanol, amylalcohol and water is from the overhead extraction of stripper 10, successively through stripper condenser 9, cooling
Device 6 is cooled to 45 DEG C, and split-phase again is carried out in rework solution liquid phase separation tank 7；
E, the waste water of 10 bottom of towe of stripper is again introduced into stripper 10 by stripper reboiler 11, it is qualified after waste water lead to
It crosses after heat exchanger 28 is cooled to 60 DEG C and is sent into sewage disposal system, dehydration rate 72%；
F, the light component in raw material is returned by crude tower condenser 2 in crude tower 3 from the tower top of crude tower 3, Ran Houyou
The overhead extraction of crude tower 3, tower top side take-off methanol, ethyl alcohol, propyl alcohol and a small amount of aqueous mixtures of crude tower 3, this part
Mixture obtains methanol product by rectifying, and ethyl alcohol, the third alcohol and water deviate from moisture by azeotropic distillation method again, then pass through rectifying
Obtain ethyl alcohol respectively, propyl alcohol product, anhydrous butanol and amylalcohol mixed alcohol are returned from the bottom of towe of crude tower 3 by rough segmentation tower reboiler 4
It returns in crude tower 3, is then produced from the bottom of towe of crude tower 3, subsequently carry out rectified purified obtaining each monomeric polyol.
Embodiment 2
A kind of process for detaching high-moisture low carbon mixed alcohol, includes the following steps：
A, first, raw material is preheated by preheater 1, control preheating temperature is 100 DEG C, and theoretical plate is entered after preheating
For number to be detached in 100 pieces of crude towers 3 to raw material, the reflux ratio of control crude tower 3 is 50, tower top pressure 100KPa,
Tower top temperature is 60 DEG C, and bottom temperature is 130 DEG C；
B, stage casing is substantially water and butanol, amylalcohol component in the tower of crude tower 3, due to water and butanol and amylalcohol it is insoluble or
Slightly soluble, by 3 recovered water of crude tower and butanol, the mixture of amylalcohol, by the alcohol phase with returning to crude tower 3 in heat exchanger 1
Heat exchange is cooled to 67 DEG C, then be cooled to 45 DEG C by cooler 6, is sent into Phase separation tank 7 together, mixture is in Phase separation
It is divided into water phase and mixing alcohol phase containing a small amount of alcohol in tank 7；
C, mixing alcohol phase is returned in crude tower 3, and the water phase containing a small amount of alcohol is exchanged heat by heat exchanger 28 to 87 DEG C first,
Into in stripper 10, the reflux ratio of control stripper 10 is 2, and tower top pressure 100KPa, tower top temperature is 85 DEG C, tower reactor temperature
Spend is 101 DEG C；
D, the azeotropic mixture of butanol, amylalcohol and water is from the overhead extraction of stripper 10, successively through stripper condenser 9, cooling
Device 6 is cooled to 45 DEG C, and split-phase again is carried out in rework solution liquid phase separation tank 7；
E, the waste water of 10 bottom of towe of stripper is again introduced into stripper 10 by stripper reboiler 11, it is qualified after waste water lead to
It crosses after heat exchanger 28 is cooled to 60 DEG C and is sent into sewage disposal system, dehydration rate 73.2%；
F, the light component in raw material is returned by crude tower condenser 2 in crude tower 3 from the tower top of crude tower 3, Ran Houyou
The overhead extraction of crude tower 3, tower top side take-off methanol, ethyl alcohol, propyl alcohol and a small amount of aqueous mixtures of crude tower 3, this part
Mixture obtains methanol product by rectifying, and ethyl alcohol, the third alcohol and water deviate from moisture by azeotropic essence gold-plating method again, then pass through rectifying
Obtain ethyl alcohol respectively, propyl alcohol product, anhydrous butanol and amylalcohol mixed alcohol are returned from the bottom of towe of crude tower 3 by rough segmentation tower reboiler 4
It returns in crude tower 3, is then produced from the bottom of towe of crude tower 3, subsequently carry out rectified purified obtaining each monomeric polyol.
The present invention is exemplarily described above, it is clear that present invention specific implementation is not subject to the restrictions described above,
As long as it employs the various improvement of inventive concept and technical scheme of the present invention progress or not improved directly applies to other fields
It closes, within protection scope of the present invention.
Claims (2)
1. a kind of process for detaching high-moisture low carbon mixed alcohol, which is characterized in that include the following steps：
A, first, raw material by preheater (1) is preheated, controls ranging from 85-100 DEG C of preheating temperature, enter after preheating
Crude tower detaches raw material in (3), reflux ratio ranging from 40-50, the tower top pressure 100KPa of control crude tower (3),
Ranging from 55-60 DEG C of tower top temperature, ranging from 125-130 DEG C of bottom temperature；
B, stage casing is substantially water and butanol, amylalcohol component in the tower of crude tower (3), since water and butanol and amylalcohol are insoluble or micro-
It is molten, by crude tower (3) recovered water and butanol, the mixture of amylalcohol, by the mixing alcohol phase with returning to crude tower (3) in heat exchanger
Heat exchange is cooled to 67 DEG C, then be cooled to 45 DEG C by cooler (6) in one (5), is sent into Phase separation tank (7) together, mixing
Object is divided into water phase and mixing alcohol phase containing a small amount of alcohol in Phase separation tank (7)；
C, mixing alcohol phase is returned in crude tower (3), and the water phase containing a small amount of alcohol is exchanged heat by heat exchanger two (8) to 87 DEG C first, then
Into in stripper (10), the reflux ratio ranging from 0.5-2 of control stripper (10), tower top pressure 100KPa, tower top temperature
Ranging from 82-85 DEG C, ranging from 100-101 DEG C of bottom temperature；
D, the azeotropic mixture of butanol, amylalcohol and water is from the overhead extractions of stripper (10), successively through stripper condenser (9), cooling
Device (6) is cooled to 45 DEG C, and split-phase again is carried out in rework solution liquid phase separation tank (7)；
E, the waste water of stripper (10) bottom of towe is again introduced into stripper (10) by stripper reboiler (11), it is qualified after waste water
Sewage disposal system is sent into after being cooled to 60 DEG C by heat exchanger two (8)；
F, the light component in raw material is returned by crude tower condenser (2) in crude tower (3) from the tower top of crude tower (3), then
By the overhead extraction of crude tower (3), tower top side take-off methanol, ethyl alcohol, propyl alcohol and a small amount of aqueous mixtures of crude tower (3),
This part mixes obtains methanol product by rectifying, and ethyl alcohol, the third alcohol and water deviate from moisture by azeotropic distillation method again, then lead to
Cross rectifying and obtain ethyl alcohol, propyl alcohol product respectively, anhydrous butanol and amylalcohol mixed alcohol from the bottom of towe of crude tower (3) by crude tower again
It boils device (4) to return in crude tower (3), then be produced from the bottom of towe of crude tower (3), subsequently carry out rectified purified obtaining each monomer
Alcohol.
2. a kind of process for detaching high-moisture low carbon mixed alcohol according to claim 1, which is characterized in that described
The number of theoretical plate of crude tower (3) is 80-100 blocks.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711348455.2A CN108129266A (en) | 2017-12-15 | 2017-12-15 | A kind of process for detaching high-moisture low carbon mixed alcohol |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711348455.2A CN108129266A (en) | 2017-12-15 | 2017-12-15 | A kind of process for detaching high-moisture low carbon mixed alcohol |
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| CN108129266A true CN108129266A (en) | 2018-06-08 |
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| CN201711348455.2A Pending CN108129266A (en) | 2017-12-15 | 2017-12-15 | A kind of process for detaching high-moisture low carbon mixed alcohol |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109369336A (en) * | 2018-12-04 | 2019-02-22 | 宁夏北控睿源再生资源有限公司 | A kind of mixed alcohol separation system |
| CN115073270A (en) * | 2022-05-12 | 2022-09-20 | 山东昆达生物科技有限公司 | Continuous azeotropic extraction and rectification method for separating low-carbon polyol-water mixture |
| CN116041150A (en) * | 2022-12-22 | 2023-05-02 | 厦门大学 | Accurate separation method of double-tower low-carbon mixed alcohol |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503771A (en) * | 2011-10-12 | 2012-06-20 | 中粮生物化学（安徽）股份有限公司 | Refining system and method of ethanol-containing aqueous solution |
| CN103193590A (en) * | 2013-03-26 | 2013-07-10 | 沈阳化工大学 | Method for continuously extracting, rectifying and separating mixed alcohols from water |
| CN104529703A (en) * | 2015-01-22 | 2015-04-22 | 神华集团有限责任公司 | Separation system and separation method of low-carbon mixed alcohol |
| CN105669377A (en) * | 2016-01-22 | 2016-06-15 | 北京凯文特科技有限公司 | Technique for separating mixed alcohol |
-
2017
- 2017-12-15 CN CN201711348455.2A patent/CN108129266A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503771A (en) * | 2011-10-12 | 2012-06-20 | 中粮生物化学（安徽）股份有限公司 | Refining system and method of ethanol-containing aqueous solution |
| CN103193590A (en) * | 2013-03-26 | 2013-07-10 | 沈阳化工大学 | Method for continuously extracting, rectifying and separating mixed alcohols from water |
| CN104529703A (en) * | 2015-01-22 | 2015-04-22 | 神华集团有限责任公司 | Separation system and separation method of low-carbon mixed alcohol |
| CN105669377A (en) * | 2016-01-22 | 2016-06-15 | 北京凯文特科技有限公司 | Technique for separating mixed alcohol |
Non-Patent Citations (1)
| Title |
|---|
| 汪多仁: "《精细化工品实用生产技术手册 增塑剂化学品生产配方和合成工艺》", 31 August 1999, 科学技术文献出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109369336A (en) * | 2018-12-04 | 2019-02-22 | 宁夏北控睿源再生资源有限公司 | A kind of mixed alcohol separation system |
| CN115073270A (en) * | 2022-05-12 | 2022-09-20 | 山东昆达生物科技有限公司 | Continuous azeotropic extraction and rectification method for separating low-carbon polyol-water mixture |
| CN115073270B (en) * | 2022-05-12 | 2024-04-02 | 山东昆达生物科技有限公司 | Continuous azeotropic extractive distillation method for separating low-carbon polyol-water mixture |
| CN116041150A (en) * | 2022-12-22 | 2023-05-02 | 厦门大学 | Accurate separation method of double-tower low-carbon mixed alcohol |
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Effective date of registration: 20210824 Address after: 300384 Room 302, door 9, block K2, Haitai green industrial base, No. 6, Haitai development road 6, Huayuan Industrial Zone, Binhai New Area, Tianjin Applicant after: Tianjin Shenlan Chemical Technology Co.,Ltd. Address before: 300384 Haitai Green Industrial Base K2-10-301, Huayuan Industrial Zone, Binhai New Area, Tianjin Applicant before: TIANJIN CHEMICAL SEPARATING TECHNOLOGIES Co.,Ltd. |
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Application publication date: 20180608 |