CN106220501A - A kind of water vapour penetration dehydration technique is for the method and apparatus of Synthesis of ethyl lactate - Google Patents
A kind of water vapour penetration dehydration technique is for the method and apparatus of Synthesis of ethyl lactate Download PDFInfo
- Publication number
- CN106220501A CN106220501A CN201610725797.0A CN201610725797A CN106220501A CN 106220501 A CN106220501 A CN 106220501A CN 201610725797 A CN201610725797 A CN 201610725797A CN 106220501 A CN106220501 A CN 106220501A
- Authority
- CN
- China
- Prior art keywords
- water
- ethyl lactate
- reactor
- rectifying column
- synthesis
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of water vapour penetration technology method and apparatus for Synthesis of ethyl lactate, belong to the application of infiltration evaporation membrance separation and organic synthesis technical field.Lactic acid in reactor, through rectification under vacuum, removes the water yield of part in lactic acid.Putting into ethanol and catalyst according to a certain ratio, after being heated to uniform temperature, reactant, under the catalytic action of catalyst, mainly generates ethyl lactate and water.In course of reaction, the upflowing vapor in reactor and descending backflow carry out heat and mass transfer in rectifying column, it is thus achieved that ethanol distillates from rectifying column tower top with water, and distillation is dehydrated as vapor permeable membrane dehydration raw material.After distillation dehydration, it is thus achieved that alcohol vapour that purity is higher is cooled to be back in reactor.The present invention uses ethanol constantly to remove with the water of generation in course of reaction as water entrainer, the water carried by raw material, promotes that reaction is moved to the direction producing ester, improves the conversion ratio of reaction, decrease later stage dewatering process.
Description
Technical field
The present invention relates to a kind of water vapour penetration dehydration technique method and apparatus for Synthesis of ethyl lactate, belong to infiltration vapour
Change membrance separation application and organic synthesis technical field.
Background technology
Ethyl lactate is one of important organic solvent, is mainly used in spice, food.This ester is as spice, modulated bright
Nurse wine, milk, butter, wine, fruit wine, Cortex cocois radicis flavor essence, for food;Can also be used for the senior solvent of olivet.
Meanwhile, or the primary organic solvent in pesticide producing, also can be used for the fields such as coating, ink, be that there is notable application prospect
Environmentally friendly solvent.In production process, main employing acid catalysis direct esterification produces ethyl lactate.This method direct reaction refluxes, process
In there is not dehydration.After reaction terminates, steam ethanol and a part of water by normal pressure;Decompression steams water and lactic acid second successively
Ester.This production process does not make processed, and in course of reaction, conversion ratio is low, and side reaction is many.On the other hand, due to aqueous in still liquid
Measuring higher, in subtractive process, after ethanol steams, a part of ethyl lactate will produce lactic acid, and this lactic acid cannot recycling.
During water is steamed by decompression, the amount of steaming of water cannot accurately control, and causes ethyl lactate loss more, and yield is relatively low.This method
The ethyl lactate finished product obtained is aqueous higher, and after the resting period is long, ethyl lactate quality reduces, and impact is normal to be used.Meanwhile,
The added value of ethyl lactate is relatively low in the market, and this process cost is higher, and benefit is relatively low.
Summary of the invention
The technical problem to be solved in the present invention is to realize carrying water in ethyl lactate synthetic reaction to move timely with generating water
Remove, it is to avoid follow-up refined during process to water, it is proposed that a kind of water vapour penetration dehydration technique is for Synthesis of ethyl lactate
Method and apparatus.The distillate distillated by reactor by rectifying column, feed pump, membrane module, cooler is carried out water vapour penetration and takes off
Water, constantly remove the water generated in the water that carries and course of reaction, it is to avoid follow-up refined during removing to water, improve
Conversion ratio and product quality, it is ensured that final products water content maintains relatively low level, prevent the reduction of product quality,
Reduce further production cost.
A kind of water vapour penetration dehydration technique, for the method for Synthesis of ethyl lactate, comprises the steps:
1st step, carries out rectification under vacuum by lactic acid, removes moisture removal, then addition ethanol and catalyst enter in a kettle. in lactic acid
Row esterification;
2nd step, the steam that esterification obtains is sent in rectifying column and is carried out rectification, obtains capital mainly containing second alcohol and water
Mixture;
3rd step, the distillation of capital is re-fed in infiltrating and vaporizing membrane being dehydrated, and the material after dehydration is back to reactor;
4th step, after reaction terminates, the still liquid of reactor first uses air-distillation to steam part ethanol, more respectively with decompression distillation
Steam ethanol and ethyl lactate.
In the 1st described step, lactic acid rectification under vacuum removes part water, and still temperature is not higher than 120 DEG C;The absolute pressure of rectification under vacuum is
100~5000Pa, make lactic acid content 92~95% after rectification.
In the 2nd described step, catalyst elects catalytic resin, concentrated sulphuric acid, p-methyl benzenesulfonic acid as.
In the 2nd described step, rectifying column tower top pressure mode of operation elects normal pressure or pressurization, preferably normal pressure as;Rectifying column tower
The reflux ratio that top uses is 0~10.
In the 3rd described step, the gauge pressure of infiltrating and vaporizing membrane feed side is 0~1Mpa;The per-meate side of infiltrating and vaporizing membrane exhausted
Pressure is 10~8000Pa.
A kind of water vapour penetration dehydration technique, for the device of Synthesis of ethyl lactate, includes reactor, on reactor top
Being provided with rectifying column, the capital of rectifying column passes sequentially through overhead condenser, ethanol receives tank, the first delivery pump, vaporizer and oozes
The feed liquid side entrance of vaporization membrane module connects thoroughly;The condensate outlet of overhead condenser is also connected with the top of rectifying column simultaneously;
It is also equipped with water on the condensate outlet of overhead condenser and receives tank and ethyl lactate reception tank;The infiltration of infiltration vaporization membrane module
Side is connected with penetrating fluid condenser, infiltration flow container successively, is also disposed with vacuum in the per-meate side of infiltration vaporization membrane module
Surge tank and vacuum pump;The feed liquid side outlet of infiltration vaporization membrane module passes sequentially through finished product cooler, product surge tank, second defeated
Pump is sent to be connected with reactor.
Install in infiltration vaporization membrane module is molecular screen membrane, chitosan film or PVA film, preferred molecular sieve film.
Beneficial effect
Compared with conventional art, the water that reaction generates can be taken off continuously by esterification reaction process of the present invention with the water carried
Remove, instead of direct condensing reflux, promote reaction process, it is to avoid the technique that subtractive process processes, reduce recovery cost,
Improve product quality, reduce production cost.This process is using ethanol as water entrainer simultaneously, can direct circulation profit after dehydration
With, decrease the discharge of ethanol;Infiltrating and vaporizing membrane material dehydration efficiency is high, can ensure higher within the shorter response time
Reaction conversion ratio;Rectifying column tower top pressure mode of operation on the reactor of the present invention is various, i.e. during pressurized operation, can realize tower
Top distillation is after partial condensation, and steam is directly entered infiltration evaporation film separation system through concurrent heating, it is to avoid double evaporation-cooling, reduces
Energy consumption;During atmospheric operation, after distillation is condensed, partial reflux, part is as the raw material of water vapour penetration film separation system, warp
After vaporizer vaporization, entering membrane module and be dehydrated, this process makes reactor and vapor permeation membrane component in operating condition side
Face is separate, easy to operate, and system is prone to stable;In later stage subtractive process, still liquid water content is low, it is to avoid the later stage is to water
Process.The film separation system dewatering efficiency of the present invention is high, and the response time is short, improves production efficiency;The membrance separation system of the present invention
In system, the Organic substance in water content of removing is less, and sewage disposal is simple, and resource recovery is high.
Accompanying drawing explanation
Fig. 1 is the vapor permeable membrane dehydration technique that provides of the present invention flow process for the method and apparatus of Synthesis of ethyl lactate
Figure: 1, reactor;2, rectifying column;3, overhead condenser;4, water receives tank;5, ethanol receives tank;6, ethyl lactate receives tank;
7, the first delivery pump;8, vaporizer;9, infiltration vaporization membrane module;10, finished product cooler;11, product surge tank;12, second is defeated
Send pump;13, penetrating fluid condenser;14, infiltration flow container;15, vacuum buffer tank;16, vacuum pump.
Detailed description of the invention
Below by detailed description of the invention, the present invention is described in further detail.But those skilled in the art will manage
Solving, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Unreceipted concrete skill in embodiment
Art or condition person, according to the technology described by the document in this area or condition or carried out according to product description.Examination used
Agent or instrument unreceipted production firm person, be can by city available from conventional products.
The value expressed using range format should be interpreted as in a flexible way not only including clearly listing as scope
The numerical value of limit value, but also include containing all single numerical value within the range or subinterval, just as each numerical value and Zi Qu
Between be expressly recited out.Such as, the concentration range of " about 0.1% to about 5% " should be understood to not only to include clearly to list
The concentration of about 0.1% to about 5%, also includes the single concentration (e.g., 1%, 2%, 3% and 4%) in the range of indication and subinterval (example
As, 0.1% to 0.5%, 1% to 2.2%, 3.3% to 4.4%).Heretofore described percentage ratio without special instruction in the case of,
Refer to percentage by weight.
" embodiment ", " another embodiment ", " embodiment " addressed in this manual etc., refer to
In conjunction with this embodiment describe specific features, structure or be included in the application generality describe at least one embodiment in.
The most multiple local appearance statement of the same race is not necessarily to refer to same embodiment.Furthermore, it is understood that combine arbitrary
When embodiment describes a specific features, structure or feature, to be advocated is to combine other embodiments to realize this spy
Levy, structure or feature also fall in the application scope of the claimed.
Water vapour penetration dewatering membrane has excellent dewatering, and water selective advantages of higher, in dehydration of organic solvent process
In show good separating property.Water vapour penetration membrane separation technique is considered as a kind of energy-efficient novel separation skill
Art, this process mainly utilizes Organic substance dissolving in film and diffusion rate to be less than water dissolving in film and diffusion, thus real
The removing of moisture in existing Organic substance.Vapor permeable membrane dehydration technique is used for the synthesis of ethyl lactate, mainly with the ethanol of excess
For water entrainer, corrosion-free, pollution-free, it is achieved the water that esterification reaction process produces removes in time, follow-up refined during will be without
Water is processed, improves the conversion ratio of reaction.
The key step of the present invention: the 1st step, carries out rectification under vacuum by lactic acid, removes moisture removal, then adds ethanol in lactic acid
Esterification is carried out in a kettle. with catalyst;2nd step, carries out rectification in the steam feeding rectifying column that esterification obtains,
Capital obtains mainly containing the mixture of second alcohol and water;3rd step, the distillation of capital is re-fed in infiltrating and vaporizing membrane taking off
Water, the material after dehydration is back to reactor;4th step, after reaction terminates, the still liquid of reactor first uses air-distillation to steam portion
Divide ethanol, then steam ethanol and ethyl lactate with decompression distillation respectively.
Wherein, lactic acid rectification under vacuum removes part water, and still temperature is not higher than 120 DEG C;The absolute pressure of rectification under vacuum be 100~
5000Pa, makes lactic acid content 92~95% after rectification, can improve reaction conversion ratio, more conducively infiltration evaporation process.
Catalyst in reaction elects catalytic resin, concentrated sulphuric acid, p-methyl benzenesulfonic acid as;In the 2nd described step, rectifying column tower top
Pressure operation mode elects normal pressure or pressurization, preferably normal pressure as;The reflux ratio that rectifying column tower top uses is 0~10.
In the 3rd described step, the gauge pressure of infiltrating and vaporizing membrane feed side is 0~1Mpa;The per-meate side of infiltrating and vaporizing membrane exhausted
Pressure is 10~8000Pa.
Apparatus structure of the present invention, as it is shown in figure 1, include reactor 1, is provided with rectification on reactor 1 top
Post 2, the capital of rectifying column 2 passes sequentially through overhead condenser 3, ethanol reception tank the 5, first delivery pump 7, vaporizer 8 and infiltration vapour
The feed liquid side entrance changing membrane module 9 connects;The condensate outlet of overhead condenser 3 the most also top with rectifying column 2 is connected;Tower
It is also equipped with water on the condensate outlet of top condenser 3 and receives tank 4 and ethyl lactate reception tank 6;Oozing of infiltration vaporization membrane module 9
Side is connected with penetrating fluid condenser 13, infiltration flow container 14 successively thoroughly, also sets gradually in the per-meate side of infiltration vaporization membrane module 9
There are vacuum buffer tank 15 and vacuum pump 16;The feed liquid side outlet of infiltration vaporization membrane module 9 passes sequentially through finished product cooler 10, finished product
Surge tank the 11, second delivery pump 12 is connected with reactor 1.
Wherein, water receives the effect of tank 4 is for receiving the moisture obtained by decompression distillation lactic raw material;Lactic acid second
It is for receiving the ethyl lactate finished product obtained after reaction terminates by distillation that ester receives tank 6.Infiltration vaporization membrane module 9 is pacified
Dress is molecular screen membrane, chitosan film or PVA film, preferred molecular sieve film.
Embodiment 1
As it is shown in figure 1, in reactor, put into 2.5kg lactic acid (aqueous about 20%), through rectification under vacuum, distillating the water yield is 0.4kg.Slightly
3.65L dehydrated alcohol and 0.04kg catalytic resin is put into after cold.After heated, under catalyst effect, carry out esterification anti-
Should, the temperature in reactor is 85 ~ 90 DEG C, and rectifying column tower top temperature controls at about 76 DEG C, wherein rectifying column height 0.8 m,
Tower diameter is about 37 mm, is filled with the glass spring filler of 3 mm × 0.5 mm specifications in rectifying column.Upflowing vapor in reactor
Carrying out heat and mass transfer in rectifying column with descending backflow, a part of overhead distillate is as backflow, and reflux ratio is 1.5,
Another part, as the material liquid of water vapour penetration dehydration, enters membrane separator group, feed liquid side after vaporizer heating vaporization
Stress control is at about 0.25MPa.This membrance separation unit is in series by 3 single tube NaA molecular sieve membrane assemblies, and membrane area is
0.09 m2, osmotic lateral pressure controls at 300Pa.The ethanol solution that purity after dehydration is higher is cooled and returned in reactor
Continue to participate in reaction and take the water that reaction generates out of;Penetrating fluid steam enters condenser under vacuum pump aspirates, to oozing after condensation
Transparent liquid storage tank is collected.It is 0.18wt.% that reaction carries out to 13.5h water content in reactor, stopped reaction, infiltration evaporation
The average operating flux of film is 1.21 kg/m2·h.Atmospheric distillation goes out part ethanol, and temperature of reaction kettle is less than 100 DEG C.Now,
Reactor liquid acid number is 3.6mg (KOH)/g, and water content is 0.12wt%;Rectification under vacuum ethanol and ethyl lactate, product acid successively
Value is about 0.8 mg (KOH)/g, and water content is 0.09wt%, and purity is 99.5%, and conversion ratio is about 98%.
Embodiment 2
As it is shown in figure 1, in reactor, put into 4kg lactic acid (aqueous about 20%), through rectification under vacuum, distillating the water yield is 0.53kg.Slightly
6.67L dehydrated alcohol and 0.032kg (accurately metering) concentrated sulphuric acid is put into after cold.After heating, carry out under catalyst effect
Esterification, the temperature in reactor is 85 ~ 90 DEG C, and rectifying column tower top temperature controls at about 76 DEG C, wherein rectifying column height
0.8 m, tower diameter are about 37 mm, are filled with the glass spring filler of 3 mm × 0.5 mm specifications in rectifying column.Upper in reactor
Rising steam and carry out heat and mass transfer in rectifying column with descending backflow, a part of overhead distillate is as backflow, reflux ratio
Being 2, another part, as the material liquid of water vapour penetration dehydration, enters membrane separator group, material after vaporizer heating vaporization
Liquid lateral pressure controls at about 0.25MPa.This membrance separation unit is in series by 4 single tube NaA molecular sieve membrane assemblies, membrane area
It is 0.12 m2, osmotic lateral pressure controls at 100Pa.The ethanol solution that purity after dehydration is higher is cooled and returned to reactor
In continue to participate in reaction and take out of reaction generate water;Penetrating fluid steam enters condenser under vacuum pump aspirates, after condensation extremely
Penetrating fluid storage tank is collected.It is 0.15wt.% that reaction carries out to 7.2h water content in reactor, stopped reaction, infiltration evaporation
The average operating flux of film is 1.15 kg/m2·h.According to the amount of sulphuric acid, accurately add 0.026kgNaOH, use acid-base neutralization
Reaction, the sulfuric acid reaction in system is complete, continue band water, after 3h hour, in reactor, water content is about 0.2wt%.Normal pressure
Rectification goes out part ethanol, and temperature of reaction kettle is less than 100 DEG C.Now, reactor liquid acid number is 2.3mg (KOH)/g, and water content is
0.073wt%;Rectification under vacuum ethanol and ethyl lactate successively, product acid number is about 0.5 mg (KOH)/g, and water content is
0.05wt%, purity is 99.6%, and conversion ratio is about 99%.
Embodiment 3
As it is shown in figure 1, in reactor, put into 3kg lactic acid (aqueous about 20%), through rectification under vacuum, distillating the water yield is 0.45kg.Slightly
4.6L dehydrated alcohol and 0.024kg (accurately metering) concentrated sulphuric acid is put into after cold.After heating, under catalyst effect, carry out ester
Changing reaction, the temperature in reactor is 85 ~ 90 DEG C, and rectifying column tower top temperature controls at about 76 DEG C, wherein rectifying column height 0.8
M, tower diameter are about 37 mm, are filled with the glass spring filler of 3 mm × 0.5 mm specifications in rectifying column.Rising in reactor is steamed
Vapour and descending backflow carry out heat and mass transfer in rectifying column, and a part of overhead distillate is as backflow, and reflux ratio is 2,
Another part, as the material liquid of water vapour penetration dehydration, enters membrane separator group, feed liquid side after vaporizer heating vaporization
Stress control is at about 0.3MPa.This membrance separation unit is in series by 4 single tube type T molecular sieve membrane modules, and membrane area is
0.12 m2, osmotic lateral pressure controls at 700Pa.The ethanol solution that purity after dehydration is higher is cooled and returned in reactor
Continue to participate in reaction and take the water that reaction generates out of;Penetrating fluid steam enters condenser under vacuum pump aspirates, to oozing after condensation
Transparent liquid storage tank is collected.It is 0.19wt.% that reaction carries out to 8.1h water content in reactor, stopped reaction, infiltrating and vaporizing membrane
Average operating flux be 1.18 kg/m2·h.According to the amount of sulphuric acid, accurately add 0.02kgNaOH, use acid-base neutralization anti-
Should, the sulfuric acid reaction in system is complete, continue band water, after 2.8h hour, in reactor, water content is about 0.21wt%.Often
Pressure rectification goes out part ethanol, and temperature of reaction kettle is less than 100 DEG C.Now, reactor liquid acid number is 2.56mg (KOH)/g, water content
For 0.1wt%;Rectification under vacuum ethanol and ethyl lactate successively, product acid number is about 0.67 mg (KOH)/g, and water content is
0.07wt%, purity is 99.3%, and conversion ratio is about 98.9%.
Embodiment 4
As it is shown in figure 1, in reactor, put into 2.5kg lactic acid (aqueous about 20%), without transmission from one meridian to another rectification under vacuum, direct plunge into
3.65L dehydrated alcohol and 0.04kg catalytic resin.After heated, under catalyst effect, carry out esterification, reactor
Interior temperature is 85 ~ 90 DEG C, and rectifying column tower top temperature controls at about 76 DEG C, and wherein rectifying column height 0.8 m, tower diameter are about 37
Mm, is filled with the glass spring filler of 3 mm × 0.5 mm specifications in rectifying column.Upflowing vapor in reactor and descending backflow
Liquid carries out heat and mass transfer in rectifying column, and a part of overhead distillate is as backflow, and reflux ratio is 1.5, and another part is made
For the material liquid of water vapour penetration dehydration, entering membrane separator group after vaporizer heating vaporization, feed liquid lateral pressure controls
About 0.25MPa.This membrance separation unit is in series by 3 single tube NaA molecular sieve membrane assemblies, and membrane area is 0.09 m2, infiltration
Lateral pressure controls at 300Pa.The ethanol solution that purity after dehydration is higher is cooled and returned in reactor continue to participate in reaction
And take the water that reaction generates out of;Penetrating fluid steam enters condenser under vacuum pump aspirates, and carries out to penetrating fluid storage tank after condensation
Collect.It is 0.18wt.% that reaction carries out to 13.5h water content in reactor, stopped reaction, the average operation of infiltrating and vaporizing membrane
Flux is 0.98 kg/m2·h.Atmospheric distillation goes out part ethanol, and temperature of reaction kettle is less than 100 DEG C.Now, reactor liquid acid number
For 5.8mg (KOH)/g, water content is 0.15wt%;Rectification under vacuum ethanol and ethyl lactate successively, product acid number is about 1 mg
(KOH)/g, water content is 0.1wt%, and purity is 99.3%, and conversion ratio is about 97%.
Claims (7)
1. the method that a water vapour penetration dehydration technique is used for Synthesis of ethyl lactate, it is characterised in that comprise the steps: the 1st
Step, carries out rectification under vacuum by lactic acid, removes moisture removal, then addition ethanol and catalyst carry out esterification instead in a kettle. in lactic acid
Should;2nd step, the steam that esterification obtains is sent in rectifying column and is carried out rectification, obtains capital mainly containing second alcohol and water
Mixture;3rd step, the distillation of capital is re-fed in infiltrating and vaporizing membrane being dehydrated, and the material after dehydration is back to reactor;
4th step, after reaction terminates, the still liquid of reactor first uses air-distillation to steam part ethanol, then steams with decompression distillation respectively
Ethanol and ethyl lactate.
Water vapour penetration dehydration technique the most according to claim 1 is for the method for Synthesis of ethyl lactate, it is characterised in that institute
In the 1st step stated, lactic acid rectification under vacuum removes part water, and still temperature is not higher than 120 DEG C;The absolute pressure of rectification under vacuum be 100~
5000Pa, makes lactic acid content 92~95% after rectification.
Water vapour penetration dehydration technique the most according to claim 1 is for the method for Synthesis of ethyl lactate, it is characterised in that institute
In the 2nd step stated, catalyst elects catalytic resin, concentrated sulphuric acid, p-methyl benzenesulfonic acid as.
Water vapour penetration dehydration technique the most according to claim 1 is for the method for Synthesis of ethyl lactate, it is characterised in that institute
In the 2nd step stated, rectifying column tower top pressure mode of operation elects normal pressure or pressurization, preferably normal pressure as;What rectifying column tower top used returns
Flow ratio is 0~10.
Water vapour penetration dehydration technique the most according to claim 1 is for the method for Synthesis of ethyl lactate, it is characterised in that institute
In the 3rd step stated, the gauge pressure of infiltrating and vaporizing membrane feed side is 0~1Mpa;The absolute pressure of the per-meate side of infiltrating and vaporizing membrane be 10~
8000Pa。
6. a water vapour penetration dehydration technique is for the device of Synthesis of ethyl lactate, it is characterised in that include reactor (1),
Be provided with rectifying column (2) on reactor (1) top, the capital of rectifying column (2) passes sequentially through overhead condenser (3), ethanol receives
Tank (5), the first delivery pump (7), vaporizer (8) are connected with the feed liquid side entrance of infiltration vaporization membrane module (9);Overhead condenser
(3) condensate outlet the most also top with rectifying column (2) is connected;It is also provided with on the condensate outlet of overhead condenser (3)
There is water to receive tank (4) and ethyl lactate receives tank (6);The per-meate side of infiltration vaporization membrane module (9) successively with penetrating fluid condenser
(13), permeate flow container (14) connection, the per-meate side of infiltration vaporization membrane module (9) is also disposed with vacuum buffer tank (15)
With vacuum pump (16);The feed liquid side outlet of infiltration vaporization membrane module (9) passes sequentially through finished product cooler (10), product surge tank
(11), the second delivery pump (12) is connected with reactor (1).
Water vapour penetration dehydration technique the most according to claim 6 is for the device of Synthesis of ethyl lactate, it is characterised in that ooze
Thoroughly install in vaporization membrane module (9) is molecular screen membrane, chitosan film or PVA film, preferred molecular sieve film.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610725797.0A CN106220501A (en) | 2016-08-25 | 2016-08-25 | A kind of water vapour penetration dehydration technique is for the method and apparatus of Synthesis of ethyl lactate |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610725797.0A CN106220501A (en) | 2016-08-25 | 2016-08-25 | A kind of water vapour penetration dehydration technique is for the method and apparatus of Synthesis of ethyl lactate |
Publications (1)
Publication Number | Publication Date |
---|---|
CN106220501A true CN106220501A (en) | 2016-12-14 |
Family
ID=57555960
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610725797.0A Pending CN106220501A (en) | 2016-08-25 | 2016-08-25 | A kind of water vapour penetration dehydration technique is for the method and apparatus of Synthesis of ethyl lactate |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN106220501A (en) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109438228A (en) * | 2018-09-28 | 2019-03-08 | 武汉三江航天固德生物科技有限公司 | The energy-saving processing technique and device of ethyl lactate |
CN109485629A (en) * | 2018-11-21 | 2019-03-19 | 浙江工业大学 | A kind of production technology of anhydrous propanone contracting glycerol |
CN111269118A (en) * | 2020-03-06 | 2020-06-12 | 滨州市华康梦之缘生物科技有限公司 | Production process of D-methyl lactate |
CN112010754A (en) * | 2020-08-19 | 2020-12-01 | 江门谦信化工发展有限公司 | Refining method for esterification synthesis of ethylene glycol methyl ether acetate |
CN113248376A (en) * | 2021-07-15 | 2021-08-13 | 山东海科新源材料科技股份有限公司 | Preparation method of electronic grade propionate, product obtained by preparation method and application of product |
CN113603585A (en) * | 2021-09-23 | 2021-11-05 | 福州大学 | Continuous production process of ultra-pure methyl lactate |
CN114377421A (en) * | 2022-02-18 | 2022-04-22 | 华陆工程科技有限责任公司 | Lactic acid oligomerization and dewatering device |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1102180A (en) * | 1993-10-28 | 1995-05-03 | 国营吴江香料厂 | new process for producing ethyl lactate |
CN1846825A (en) * | 2002-02-08 | 2006-10-18 | 阿托菲纳公司 | Method for lactic acid oligomerization |
CN104262140A (en) * | 2014-09-22 | 2015-01-07 | 江苏九天高科技股份有限公司 | Method and device for producing diethyl maleate by virtue of rectification and steam osmosis coupling |
CN104926655A (en) * | 2015-06-11 | 2015-09-23 | 江苏九天高科技股份有限公司 | Technology and device for diethyl oxalate synthesis through vapor permeation dehydration process |
CN104926653A (en) * | 2015-06-11 | 2015-09-23 | 江苏九天高科技股份有限公司 | Reaction and steam osmotic dehydration coupled ethyl hexanoate synthesizing process and device |
CN104945249A (en) * | 2015-06-11 | 2015-09-30 | 江苏九天高科技股份有限公司 | Method and device for producing ethyl formate through reactive distillation and steam osmosis membrane coupling |
-
2016
- 2016-08-25 CN CN201610725797.0A patent/CN106220501A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1102180A (en) * | 1993-10-28 | 1995-05-03 | 国营吴江香料厂 | new process for producing ethyl lactate |
CN1846825A (en) * | 2002-02-08 | 2006-10-18 | 阿托菲纳公司 | Method for lactic acid oligomerization |
CN104262140A (en) * | 2014-09-22 | 2015-01-07 | 江苏九天高科技股份有限公司 | Method and device for producing diethyl maleate by virtue of rectification and steam osmosis coupling |
CN104926655A (en) * | 2015-06-11 | 2015-09-23 | 江苏九天高科技股份有限公司 | Technology and device for diethyl oxalate synthesis through vapor permeation dehydration process |
CN104926653A (en) * | 2015-06-11 | 2015-09-23 | 江苏九天高科技股份有限公司 | Reaction and steam osmotic dehydration coupled ethyl hexanoate synthesizing process and device |
CN104945249A (en) * | 2015-06-11 | 2015-09-30 | 江苏九天高科技股份有限公司 | Method and device for producing ethyl formate through reactive distillation and steam osmosis membrane coupling |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109438228A (en) * | 2018-09-28 | 2019-03-08 | 武汉三江航天固德生物科技有限公司 | The energy-saving processing technique and device of ethyl lactate |
CN109485629A (en) * | 2018-11-21 | 2019-03-19 | 浙江工业大学 | A kind of production technology of anhydrous propanone contracting glycerol |
CN111269118A (en) * | 2020-03-06 | 2020-06-12 | 滨州市华康梦之缘生物科技有限公司 | Production process of D-methyl lactate |
CN112010754A (en) * | 2020-08-19 | 2020-12-01 | 江门谦信化工发展有限公司 | Refining method for esterification synthesis of ethylene glycol methyl ether acetate |
CN112010754B (en) * | 2020-08-19 | 2023-02-28 | 江门谦信化工发展有限公司 | Refining method for esterification synthesis of ethylene glycol methyl ether acetate |
CN113248376A (en) * | 2021-07-15 | 2021-08-13 | 山东海科新源材料科技股份有限公司 | Preparation method of electronic grade propionate, product obtained by preparation method and application of product |
CN113603585A (en) * | 2021-09-23 | 2021-11-05 | 福州大学 | Continuous production process of ultra-pure methyl lactate |
CN114377421A (en) * | 2022-02-18 | 2022-04-22 | 华陆工程科技有限责任公司 | Lactic acid oligomerization and dewatering device |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN106220501A (en) | A kind of water vapour penetration dehydration technique is for the method and apparatus of Synthesis of ethyl lactate | |
CN206033624U (en) | Vapor permeation dehydration techniques is used for synthetic ethyl lactate's device | |
CN103071307A (en) | Rectification-steam penetration-coupled organic solvent dewatering method and device | |
CN107628946A (en) | The method and device of reactive distillation film device coupling production ethyl acetate in high purity | |
CN104926653A (en) | Reaction and steam osmotic dehydration coupled ethyl hexanoate synthesizing process and device | |
CN107739301B (en) | Polymethoxy dimethyl ether synthesis system and process | |
CN104557529A (en) | Refining method and device for n-propyl acetate esterification synthesis | |
CN104262140A (en) | Method and device for producing diethyl maleate by virtue of rectification and steam osmosis coupling | |
CN104370698A (en) | Process for separating dimethyl carbonate and methanol by employing pervaporation and pressure distillation integration | |
CN108863719A (en) | Steam infiltration-alkaline process coupling prepares the method and device of sodium methoxide | |
CN106243068A (en) | A kind of method by coupling rectification purification of tetrahydrofuran | |
CN106674043A (en) | Device and method for preparing high-purity acetonitrile by ammoniation of acetic acid | |
CN103342642A (en) | Process for continuously producing dimethyl adipate through reaction-rectification method | |
CN104370699B (en) | The technique of the integrated separating dimethyl carbonate of a kind of infiltration evaporation-atmospheric distillation and methyl alcohol | |
CN104945249A (en) | Method and device for producing ethyl formate through reactive distillation and steam osmosis membrane coupling | |
CN209243063U (en) | A kind of resource utilization system of brewed spirit by-product yellow water | |
CN101985349A (en) | Production method for preparing deuterium depleted water | |
CN106518683A (en) | Method and device for synthesizing triethyl citrate by applying vapor permeation dehydration technique | |
CN106431884A (en) | Device and method for preparing butyric acid through butyraldehyde oxidation | |
CN209210671U (en) | Steam infiltration-alkaline process coupling prepares the device of sodium methoxide | |
CN206188686U (en) | Device of butyraldehyde oxidation preparation butyric acid | |
CN206279107U (en) | A kind of Steam soak dehydration technique is used for the device of synthesizing citric acid triethyl | |
CN213724893U (en) | Ethanol distillation pilot system | |
JP2009073793A (en) | System for separating and concentrating ethanol | |
CN204211671U (en) | The device of ethyl maleate is produced in a kind of rectifying-water vapour penetration coupling |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161214 |
|
RJ01 | Rejection of invention patent application after publication |