CN105732321A - Rectification enriching device for 1, 3-propylene glycol - Google Patents
Rectification enriching device for 1, 3-propylene glycol Download PDFInfo
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- CN105732321A CN105732321A CN201610243735.6A CN201610243735A CN105732321A CN 105732321 A CN105732321 A CN 105732321A CN 201610243735 A CN201610243735 A CN 201610243735A CN 105732321 A CN105732321 A CN 105732321A
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- tower
- removing column
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- column
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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 invention relates to a rectification enriching device for 1, 3-propylene glycol and mainly aims at solving the problems that in the prior art, an extraction agent needs to be used, energy consumption is high, and the process is complicated.The rectification enriching device for 1, 3-propylene glycol mainly comprises a light component removal tower and a heavy component removal tower.A fermentation liquid feeding pipeline is arranged at the position from the 10th tower plate to the 20th tower plate from top to bottom of the light component removal tower.A tower reactor flow pipeline of the light component removal tower is connected with a feeding pipeline of the heavy component removal tower.The feeding position of the heavy component removal tower is from the 15th tower plate to the 25th tower plate from top to bottom of the heavy component removal tower.A 1, 3-propylene glycol product flow pipeline is arranged on the top of the heavy component removal tower.According to the operation conditions of the light component removal tower, the number of the tower plates ranges from 20 to 40, the tower top temperature ranges from 45 DEG C to 65 DEG C, the tower reactor temperature ranges from 155 DEG C to 175 DEG C, and the operation pressure ranges from 5 kPa to 25 kPa.According to the operation conditions of the heavy component removal tower, the number of the tower plates ranges from 20 to 40, the tower top temperature ranges from 125 DEG C to 145 DEG C, the tower reactor temperature ranges from 165 DEG C to 185 DEG C, and the operation pressure ranges from 1 kPa to 15 kPa.According to the technical scheme, the problems are well solved, and the rectification enriching device can be applied to production of 1, 3-propylene glycol.
Description
Technical field
The present invention relates to the rectification concentration unit of a kind of 1,3-propylene glycol.
Background technology
1,3-PD is the Novel chemical raw material of a kind of great potential, is manufacturing polyester fiber, polyurethane, PUR, powder
The aspects such as end coating, antifreeze, packaging material and organic synthesis intermediate suffer from being widely applied, and wherein manufacture high property
The polyester one polytrimethylene terephthalate (PTT) of energy is purposes currently mainly.1,3-propylene glycol can pass through chemical method road
Line and bioanalysis route produce, and wherein use biotechnology to produce 1,3-PD, are characterized with its Green Chemistry, have anti-
Answer the feature such as mild condition, easy and simple to handle, by-product is few, environmental pollution is little, available regenerated resources, become new century raw
One of focus of thing chemical research.
Currently manufactured high performance polyester fiber PTT is the purposes that 1,3-PD is main, and 1,3-PD quality is for PTT
Resin has large effect, and its moderate purity is maximum on the impact of PTT resin, is a main quality of concern.When
When 1,3-PD purity is less than 99.5wt%, the intrinsic viscosity of resin just cannot improve, thus affects the serviceability of resin.
Use biofermentation legal system 1,3-PD, fermentation liquid there is also the by-products such as ethanol, 2,3-butanediol, butanoic acid, acetic acid
Thing and thalline and remaining culture medium etc..Separating and extracting 1,3-propanediol from fermentation liquid the most efficiently at low cost
Become this area study hotspot.
Patent CN1417185A and CN1417184A disclose the method for refined purifying 1,3-propylene glycol, pass through respectively
Anion exchange resin and catalyzing cation exchange resin reaction reduce impurity content therein.These methods are to a certain degree
On can improve the concentration of 1,3-PD, but its be primarily directed to aldehyde in the 1,3-PD that chemical method produces too high and
The measure taked, reduces the aldehyde in product by chemical reaction, to improve its colourity.The 1,3-that bioanalysis is produced
The 1,3-propylene glycol effect inconspicuous that propylene glycol especially by-product glycerol of biological diesel oil produces.Due to bioanalysis 1,3-propylene glycol
Aldehyde the highest, but other impurity component is increasingly complex.
Patent CN1460671A proposes a kind of method separating and recovering 1,3-PD from fermentation liquid, and specific practice is band
The fermentation liquid direct evaporation of bacterium is concentrated to the 1/2～1/20 of original volume, add a certain proportion of alcohols solvent such as methanol, ethanol,
Propanol or acetone etc., filter or centrifugal obtain clear liquid, and after distillating recovering solvent, then rectification under vacuum obtains product 1,3-PD.
This method is the existence of suitable water owing to concentrated solution also has, and solvent used is all hydrophilic, and thalline and albumen etc. are at this
Plant the character in alcohol (ketone) aqueous systems and for there to be big change, be centrifuged or filtration sterilization is the most difficult, the clear liquid obtained
Color is relatively deep, and present in fermentation liquid, impurity is not completely removed.
Patent CN 102816048A proposes a kind of method of extract and separate 1,3-propylene glycol from fermentation liquid: will contain 1,3-the third two
The fermentation liquid of alcohol directly contacts the steps such as extraction, extractant regeneration and product rectification in extraction tower with composite extractant, completes
Isolated and purified 1,3-propylene glycol from fermentation liquid.Its extractant used is the fatty alcohol of C4～C6, can, in aqueous
With 1,3-PD, there is hydrogen bond action, 1,3-PD is had preferable partition coefficient, be preferable extractant.Use this
Method energy, can reduce energy consumption to a certain extent, and extractant is easier to regeneration and uses, cost-effective.But its shortcoming is water to exist
Fatty alcohol has certain dissolubility, after multitple extraction, fermentation liquid has a lot of water and enters in extraction phase fatty alcohol,
Also the salt in fermentation liquid is brought in extraction phase simultaneously, adds complexity and the energy consumption of later separation.
Summary of the invention
The technical problem to be solved be prior art needs to use extractant, energy consumption be higher, the asking of complex process
Topic, it is provided that the rectification concentration unit of a kind of new 1,3-PD.This device, in the production of 1,3-PD, has nothing
Need to use that extractant, energy consumption be relatively low, the simple advantage of technique.
For solving the problems referred to above, the technical solution used in the present invention is as follows: the rectification concentration unit of a kind of 1,3-PD, main
Lightness-removing column to be included and weight-removing column, be provided with fermentation liquid feeding line at the several 10th～20 block of column plate of lightness-removing column, de-
Light tower tower reactor logistic pipeline is connected with the feeding line of weight-removing column, and the feed entrance point of described weight-removing column is positioned at several the
At 15～25 blocks of column plates, weight-removing column tower top is provided with 1,3-PD product stream pipeline；Wherein, the operation bar of described lightness-removing column
Part is: the number of plates 20～40, tower top temperature 45～65 DEG C, bottom temperature 155～175 DEG C, operates pressure 5～25kPa；
The operating condition of described weight-removing column is: the number of plates 20～40, tower top temperature 125～145 DEG C, bottom temperature 165～185 DEG C,
Operation pressure 1～15kPa；In described fermentation liquid, 1,3-PD concentration is 60～80wt%, and described 1,3-PD product is dense
Degree is 99.5wt%.
In technique scheme, it is preferable that the operating condition of described lightness-removing column is: the number of plates 25～35, tower top temperature 50～
60 DEG C, bottom temperature 160～170 DEG C, operate pressure 10～20kPa, feedboard position numerical digit from top to bottom is in the 12nd～16
At block column plate；The operating condition of described weight-removing column is: the number of plates 25～35, tower top temperature 130～140 DEG C, bottom temperature
170～180 DEG C, operating pressure 5～10kPa, feedboard position numerical digit from top to bottom is at the 18th～23 block of column plate.
In technique scheme, it is preferable that the 1,3-PD concentration in described fermentation liquid is 65～75wt%.
In technique scheme, it is preferable that it is 60～80wt% that described fermentation liquid obtains 1,3-PD concentration after slightly evaporating
Fermentation liquid enter lightness-removing column.
In technique scheme, it is preferable that in described lightness-removing column tower reactor logistics, the concentration of 1,3-PD is 93～98wt%.
This patent uses the method for continuous rectification, it is to avoid in purification process catalyst or the use of extractant, decreases dirt
The generation of dye thing, simplifies technical process, has saved energy consumption, guarantees that the 1,3-PD of output can meet production high-quality simultaneously
The requirement of amount new polyester PTT, achieves preferable technique effect.
Accompanying drawing explanation
Fig. 1 is the structural representation of device of the present invention.
In Fig. 1, T1 is lightness-removing column, and T2 is weight-removing column；1 is feed stream, and 2 is lightness-removing column overhead stream, and 3 for de-light
Tower tower reactor logistics, 4 is 1,3-PD product stream, and 5 is weight-removing column tower reactor logistics.
Below by embodiment, the invention will be further elaborated, but is not limited only to the present embodiment.
Detailed description of the invention
[embodiment 1]
The rectification concentration unit of a kind of 1,3-PD, mainly includes lightness-removing column and weight-removing column, lightness-removing column tower reactor logistic pipeline with
The feeding line of weight-removing column is connected, and weight-removing column tower top is provided with 1,3-PD product stream pipeline.
The 1,3-PD material that content is 75wt% from Cu Liu workshop section enters in the middle part of lightness-removing column, obtains at lightness-removing column top
Water content is the waste liquid of 90wt%, obtains the process-stream that 1,3-PD concentration is 95.3wt% bottom lightness-removing column；From
High concentration 1,3-PD process stream bottom lightness-removing column enters weight-removing column bottom, obtains 1,3-PD at weight-removing column top
Concentration is the product stream of 99.5wt%, and tower top obtains the waste liquid containing glycerol, diethylene glycol etc..
The lightness-removing column number of plates is 30, and feed entrance point is that at several 14th block of column plate, operation pressure is 15kPa, tower
Top temperature is 54 DEG C, and bottom temperature is 167 DEG C；The weight-removing column number of plates is 32, and feed entrance point is the 22nd piece of tower from top to bottom
At plate, operation pressure is 6kPa, and tower top temperature is 134 DEG C, and bottom temperature is 176 DEG C.
The 1,3-propylene glycol product obtained disclosure satisfy that the requirement producing high-quality new polyester PTT.
[embodiment 2]
The 1,3-PD material that content is 80wt% from Cu Liu workshop section enters in the middle part of lightness-removing column, obtains at lightness-removing column top
Water content is the waste liquid of 90wt%, obtains the process-stream that 1,3-PD concentration is 96.2wt% bottom lightness-removing column；From
High concentration 1,3-PD process stream bottom lightness-removing column enters weight-removing column bottom, obtains 1,3-PD at weight-removing column top
Concentration is the product stream of 99.5wt%, and tower top obtains the waste liquid containing glycerol, diethylene glycol etc..
The lightness-removing column number of plates is 28, and feed entrance point is that at several 10th block of column plate, operation pressure is 12kPa, tower
Top temperature is 48 DEG C, and bottom temperature is 155 DEG C；The weight-removing column number of plates is 30, and feed entrance point is the 18th piece of tower from top to bottom
At plate, operation pressure is 5kPa, and tower top temperature is 129 DEG C, and bottom temperature is 170 DEG C.
The 1,3-propylene glycol product obtained disclosure satisfy that the requirement producing high-quality new polyester PTT.
[embodiment 3]
The 1,3-PD material that content is 70wt% from Cu Liu workshop section enters in the middle part of lightness-removing column, obtains at lightness-removing column top
Water content is the waste liquid of 90wt%, obtains the process-stream that 1,3-PD concentration is 94.6wt% bottom lightness-removing column；From
High concentration 1,3-PD process stream bottom lightness-removing column enters weight-removing column bottom, obtains 1,3-PD at weight-removing column top
Concentration is the product stream of 99.5wt%, and tower top obtains the waste liquid containing glycerol, diethylene glycol etc..
The lightness-removing column number of plates is 32, and feed entrance point is that at several 15th block of column plate, operation pressure is 18kPa, tower
Top temperature is 62 DEG C, and bottom temperature is 175 DEG C；The weight-removing column number of plates is 32, and feed entrance point is the 24th piece of tower from top to bottom
At plate, operation pressure is 8kPa, and tower top temperature is 136 DEG C, and bottom temperature is 180 DEG C.
The 1,3-propylene glycol product obtained disclosure satisfy that the requirement producing high-quality new polyester PTT.
[embodiment 4]
The 1,3-PD material that content is 60wt% from Cu Liu workshop section enters in the middle part of lightness-removing column, obtains at lightness-removing column top
Water content is the waste liquid of 90wt%, obtains the process-stream that 1,3-PD concentration is 93.5wt% bottom lightness-removing column；From
High concentration 1,3-PD process stream bottom lightness-removing column enters weight-removing column bottom, obtains 1,3-PD at weight-removing column top
Concentration is the product stream of 99.5wt%, and tower top obtains the waste liquid containing glycerol, diethylene glycol etc..
The lightness-removing column number of plates is 40, and feed entrance point is that at several 19th block of column plate, operation pressure is 8kPa, tower top
Temperature is 46 DEG C, and bottom temperature is 156 DEG C；The weight-removing column number of plates is 38, and feed entrance point is the 24th block of column plate from top to bottom
Place, operation pressure is 2kPa, and tower top temperature is 126 DEG C, and bottom temperature is 167 DEG C.
The 1,3-propylene glycol product obtained disclosure satisfy that the requirement producing high-quality new polyester PTT.
[embodiment 5]
The 1,3-PD material that content is 65wt% from Cu Liu workshop section enters in the middle part of lightness-removing column, obtains at lightness-removing column top
Water content is the waste liquid of 90wt%, obtains the process-stream that 1,3-PD concentration is 94.2wt% bottom lightness-removing column；From
High concentration 1,3-PD process stream bottom lightness-removing column enters weight-removing column bottom, obtains 1,3-PD at weight-removing column top
Concentration is the product stream of 99.5wt%, and tower top obtains the waste liquid containing glycerol, diethylene glycol etc..
The lightness-removing column number of plates is 22, and feed entrance point is that at several 9th block of column plate, operation pressure is 23kPa, tower top
Temperature is 64 DEG C, and bottom temperature is 175 DEG C；The weight-removing column number of plates is 20, and feed entrance point is the 14th block of column plate from top to bottom
Place, operation pressure is 14kPa, and tower top temperature is 142 DEG C, and bottom temperature is 180 DEG C.
The 1,3-propylene glycol product obtained disclosure satisfy that the requirement producing high-quality new polyester PTT.
[embodiment 6]
The 1,3-PD material that content is 75wt% from Cu Liu workshop section enters in the middle part of lightness-removing column, obtains at lightness-removing column top
Water content is the waste liquid of 90wt%, obtains the process-stream that 1,3-PD concentration is 95.0wt% bottom lightness-removing column；From
High concentration 1,3-PD process stream bottom lightness-removing column enters weight-removing column bottom, obtains 1,3-PD at weight-removing column top
Concentration is the product stream of 99.5wt%, and tower top obtains the waste liquid containing glycerol, diethylene glycol etc..
The lightness-removing column number of plates is 20, and feed entrance point is that at several 8th block of column plate, operation pressure is 25kPa, tower top
Temperature is 65 DEG C, and bottom temperature is 175 DEG C；The weight-removing column number of plates is 40, and feed entrance point is the 26th block of column plate from top to bottom
Place, operation pressure is 3kPa, and tower top temperature is 127 DEG C, and bottom temperature is 178 DEG C.
The 1,3-propylene glycol product obtained disclosure satisfy that the requirement producing high-quality new polyester PTT.
Claims (5)
1. a rectification concentration unit for 1,3-PD, mainly includes lightness-removing column and weight-removing column, lightness-removing column the several 10th～
Being provided with fermentation liquid feeding line at 20 blocks of column plates, lightness-removing column tower reactor logistic pipeline is connected with the feeding line of weight-removing column, described de-
The feed entrance point of weight tower is positioned at several 15th～25 block of column plate, and weight-removing column tower top is provided with 1,3-PD product thing
Flow tube line；Wherein, the operating condition of described lightness-removing column is: the number of plates 20～40, tower top temperature 45～65 DEG C, tower reactor temperature
Spend 155～175 DEG C, operate pressure 5～25kPa；The operating condition of described weight-removing column is: the number of plates 20～40, tower top temperature
Spend 125～145 DEG C, bottom temperature 165～185 DEG C, operate pressure 1～15kPa；In described fermentation liquid, 1,3-propylene glycol is dense
Degree is 60～80wt%, and described 1,3-PD product design is 99.5wt%.
The rectification concentration unit of 1,3-PD the most according to claim 1, it is characterised in that the operating condition of described lightness-removing column
For: the number of plates 25～35, tower top temperature 50～60 DEG C, bottom temperature 160～170 DEG C, operate pressure 10～20kPa,
Feedboard position numerical digit from top to bottom is at the 12nd～16 block of column plate；The operating condition of described weight-removing column is: the number of plates 25～
35, tower top temperature 130～140 DEG C, bottom temperature 170～180 DEG C, operate pressure 5～10kPa, feedboard position is from upper
To lower numerical digit at the 18th～23 block of column plate.
The rectification concentration unit of 1,3-PD the most according to claim 1, it is characterised in that 1 in described fermentation liquid, 3-the third two
Determining alcohol is 65～75wt%.
The rectification concentration unit of 1,3-PD the most according to claim 1, it is characterised in that described fermentation liquid is after slightly evaporating
Obtain the fermentation liquid that 1,3-PG concentration is 60～80wt% and enter lightness-removing column.
The rectification concentration unit of 1,3-PD the most according to claim 1, it is characterised in that in described lightness-removing column tower reactor logistics
The concentration of 1,3-propylene glycol is 93～98wt%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610243735.6A CN105732321A (en) | 2016-04-19 | 2016-04-19 | Rectification enriching device for 1, 3-propylene glycol |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610243735.6A CN105732321A (en) | 2016-04-19 | 2016-04-19 | Rectification enriching device for 1, 3-propylene glycol |
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| CN105732321A true CN105732321A (en) | 2016-07-06 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112920020A (en) * | 2021-01-29 | 2021-06-08 | 浙江恒澜科技有限公司 | Refining production line and method of 1, 3-propylene glycol |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1816629A (en) * | 2003-05-06 | 2006-08-09 | 纳幕尔杜邦公司 | Purification of biologically-produced 1,3-propanediol |
| CN101260026A (en) * | 2008-04-16 | 2008-09-10 | 上海华谊丙烯酸有限公司 | Purification method of preparing 1,2-propylene glycol by glycerine hydrogenation |
| CN103667365A (en) * | 2012-08-31 | 2014-03-26 | 郸城财鑫糖业有限责任公司 | Method for preparing dihydric alcohol from crop straw |
-
2016
- 2016-04-19 CN CN201610243735.6A patent/CN105732321A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1816629A (en) * | 2003-05-06 | 2006-08-09 | 纳幕尔杜邦公司 | Purification of biologically-produced 1,3-propanediol |
| CN101260026A (en) * | 2008-04-16 | 2008-09-10 | 上海华谊丙烯酸有限公司 | Purification method of preparing 1,2-propylene glycol by glycerine hydrogenation |
| CN103667365A (en) * | 2012-08-31 | 2014-03-26 | 郸城财鑫糖业有限责任公司 | Method for preparing dihydric alcohol from crop straw |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112920020A (en) * | 2021-01-29 | 2021-06-08 | 浙江恒澜科技有限公司 | Refining production line and method of 1, 3-propylene glycol |
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