CN110283071A - A kind of system and method based on micro passage reaction synthesis of oxalic acid methyl ethyl ester - Google Patents
A kind of system and method based on micro passage reaction synthesis of oxalic acid methyl ethyl ester Download PDFInfo
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- CN110283071A CN110283071A CN201910557883.9A CN201910557883A CN110283071A CN 110283071 A CN110283071 A CN 110283071A CN 201910557883 A CN201910557883 A CN 201910557883A CN 110283071 A CN110283071 A CN 110283071A
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- microchannel
- entrance
- micro passage
- oxalate
- methyl ethyl
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/03—Preparation of carboxylic acid esters by reacting an ester group with a hydroxy group
Abstract
The invention belongs to organic synthesis field, especially a kind of system and method based on micro passage reaction synthesis of oxalic acid methyl ethyl ester.System includes the first stock bottle, the second stock bottle, micro passage reaction, collection device；The micro passage reaction includes first entrance microchannel, second entrance microchannel, microchannel and channel outlet, the first entrance microchannel and second entrance microchannel are connect with the first stock bottle and the second stock bottle respectively, first entrance microchannel, the second entrance microchannel other end are connect with microchannel, and channel outlet is connect with collection device.The yield of the available higher methyl ethyl oxalate of method of transesterification is used using the efficient mixing of microreactor, process intensification, and its selectivity is also higher；Compared to traditional sustainable charging of tank reactor microreactor, the production efficiency of product is greatly improved, and process safety is controllable, reduces the generation of human accident.
Description
Technical field
The invention belongs to organic synthesis field, especially a kind of system based on micro passage reaction synthesis of oxalic acid methyl ethyl ester
And method.
Background technique
Oxalic acid ester is a kind of important industrial chemicals and medicine intermediate, such as diethy-aceto oxalate (Diethyl
Oxalate, vehicle economy O), dimethyl oxalate (Dimethyl Oxalate, abbreviation DMO) all can be used as intermediate synthetic drug sulphur
Amine first oxazole plastics promotor (Transesterification of diethyl oxalate with phenol using
285,1-2,190-195 of MoO3/SiO2 catalyst.Applied Catalysis A:General.2005), among dyestuff
Body；The pilot process that ethylene glycol is prepared using synthesis gas is exactly to need first synthesis of oxalate, then uses hydrogenation of oxalate for preparing again
Standby pure ethylene glycol patent (CN106083522A), it is sufficient to illustrate that oxalate is a kind of important source material and also in coal chemical industry product
In applied.
Therefore, the intermediate material as DEO and DMO, methyl ethyl oxalate (Ethyl Methyl Oxalate, abbreviation EMO,
It is a kind of colorless and transparent liquid, fusing point: -42.88 DEG C, boiling point: 157.29 DEG C), diethy-aceto oxalate decarbonylation prepares carbonic acid diethyl
Ester (Gas phase decarbonylation of diethyl oxalate to diethyl carbonate over
alkali-containing catalyst.Journal of Molecular Catalysis A:Chemical 2009,
306,130-135), then equally methyl ethyl carbonate can be prepared with methyl ethyl oxalate decarbonylation.And carbonates are applied in battery electricity
The application such as liquid, polymer is solved, therefore can be used as the intermediate of its synthesis as oxalate, thus it is answered for oxalate
It has a extensive future.Since three kinds of structures of matter are similar, their property is also extremely similar, and because methyl ethyl oxalate has not
It is same as the asymmetry structure of dimethyl oxalate and diethy-aceto oxalate, contains methyl and ethyl simultaneously, shows polar state, compare carbon
Sour methyl ethyl ester lacks a carbonyl, it also can be used as solvent and uses (patent CN101289395A).
The synthetic method of synthesis and diethy-aceto oxalate in view of methyl ethyl carbonate, may synthesis of oxalic acid there is several methods that synthesizing
Methyl ethyl ester has CO catalysis coupling to prepare the preparation such as transesterification of oxalate, oxalic acid and alcohol esterification and oxalate.
These methods mostly carry out in traditional tank reactor, and the preparation production cycle is long, preparation process is complicated, unit consumption
Height largely effects on combined coefficient.And be substantially shorter the production cycle for synthesizing in microreactor, continuous-stable into
Material, process can be strengthened, and also relatively simple easy tune, combined coefficient can improve process conditions by a relatively large margin.
The synthetic reaction equation of methyl ethyl oxalate:
(1)
Microreactor is micromation reaction system, and bulk properties size reduction is to 1000 μm~10 μm.Microreactor provides
Lesser diffusion length and biggish surface-to-volume ratio (10000~50000m2m-3), so as to cause higher heat transfer
Rate and mass transfer rate (Biodiesel production in micro-reactors:A review, Energy for
Sustainable Development,2018,43,143-161).Therefore technical process reinforcing shows outstanding performance,
Organic synthesis field yields unusually brilliant results.Due to its good security control, microreactor has in diazotising, nitrification etc. is widely answered
With.Compared to traditional tank reactor, the application of micro passage reaction is so that reaction solution progress height mixing, greatly shortens anti-
Between seasonable, so that reaction is more efficient, production reaction process is safer, process conditions are easier to accuracy controlling and optimization, improves reaction
Selectivity and product yield.
Summary of the invention
Technical problem solved by the invention is to provide a kind of is based on micro passage reaction synthesis of oxalic acid methyl ethyl ester
System and method.
The technical solution for realizing the aim of the invention is as follows:
A kind of system based on micro passage reaction synthesis of oxalic acid methyl ethyl ester, including the first stock bottle, the second stock bottle are micro-
Channel reactor, collection device；
The micro passage reaction includes first entrance microchannel, second entrance microchannel, microchannel and channel outlet, institute
It states first entrance microchannel and second entrance microchannel to connect with the first stock bottle and the second stock bottle respectively, first entrance is micro- logical
Road, the second entrance microchannel other end are connect with microchannel, and the channel outlet is connect with collection device.
Further, it is connected between first stock bottle and first entrance microchannel by the first infusion pump, described the
It is connected between two stock bottles and second entrance microchannel by the second infusion pump.
Further, the capsule shape rubber grain of periodic arrangement, two parallel rubber are embedded with above the microchannel
Grain at an angle, to be divided into thread to mix two strands of materials.
Further, the micro passage reaction further includes lower substrate, upper substrate, the first entrance microchannel, second
Inlet microchannel, microchannel and channel outlet are arranged on lower substrate.
Further, temperature control device is set on the upper substrate.
It further, further include gas-chromatography, production fluid bottle rear end connects gas-chromatography.
A method of using above-mentioned system synthesis methyl ethyl oxalate, include the following steps:
(1) diethy-aceto oxalate and methanol feed liquid is respectively configured；
(2) diethy-aceto oxalate and methanol solution are passed through into high pressure pump feed liquor respectively, solution is pumped by high pressure pump
Pressure effect infusion enters the two entrances of micro passage reaction；It is adjusted by the temperature control device of micro passage reaction upper substrate anti-
Temperature is answered, esterification is carried out；
(3) it is flowed into collection device via channel outlet, then detects the yield of methyl ethyl oxalate by gas-chromatography.
Further, reaction solution is controlled in microchannel by controlling the feed flow rate of two kinds of materials in the step (2)
The flow velocity of reaction time in reactor, catalyst methanol solution flow velocity and diethy-aceto oxalate is respectively 5 μ of μ L/min~30
L/min, 5 μ of μ L/min~30 L/min；Reaction temperature is 20 DEG C~50 DEG C.
Further, the overall flow rate is to be changed under 10 μ of μ L/min~60 L/min by changing two bursts of feed flow rates
The molar ratio of methanol and diethy-aceto oxalate, molar ratio range are 1.3:1~5:1.
Further, the catalyst type in the catalyst methanol is KOH, K2CO3、KHCO3Or CH3OK, catalyst are dense
Degree is 5mg/mL~20mg/mL.
Compared with prior art, the present invention its remarkable advantage is as follows:
(1) the available higher oxalic acid of method of transesterification is used using the efficient mixing of microreactor, process intensification
The yield of methyl ethyl ester, and its selectivity is also higher；Compared to traditional sustainable charging of tank reactor microreactor, greatly mention
The production efficiency of high product, and process safety is controllable, reduces the generation of human accident.
(2) heating device on upper substrate is heated using galvanic couple, and has temperature sensor, can accurate temperature control.
(3) high pressure pump can change in turn the molar ratio of reactant and stopping for reaction progress with accuracy controlling flow velocity
Stay the time.
Present invention is further described in detail with reference to the accompanying drawing.
Detailed description of the invention
Fig. 1 is the system schematic that methyl ethyl oxalate is prepared based on micro passage reaction.
Fig. 2 is the upper substrate and heating device of microreactor.
Fig. 3 is conversion ratio shadow of 1 feed flow rate of embodiment to the selectivity of methyl ethyl oxalate, yield and diethy-aceto oxalate
It rings.
Fig. 4 is conversion ratio shadow of 2 reaction temperature of embodiment to the selectivity of methyl ethyl oxalate, yield and diethy-aceto oxalate
It rings.
Fig. 5 is that 3 reaction raw materials molar ratio of embodiment turns the selectivity of methyl ethyl oxalate, yield and diethy-aceto oxalate
Rate influences.
Fig. 6 is conversion ratio of 4 catalyst concn of embodiment to the selectivity of methyl ethyl oxalate, yield and diethy-aceto oxalate
It influences.
Fig. 7 is to carry out the production fluid of 6 secondary responses under preferable reaction condition, the selectivity of methyl ethyl oxalate, yield with
And the conversion ratio test result of diethy-aceto oxalate.
Description of symbols:
The first stock bottle of 1-, the second stock bottle of 2-, the first infusion pump of 3-, the second infusion pump of 4-, 5- first entrance microchannel,
6- second entrance microchannel, 7- rubber grain, the microchannel 8-, 9- lower substrate, 10- channel outlet, 11- collection device, 12- gas phase
Chromatography, 13- temperature control device, 14- upper substrate.
Specific embodiment
The present invention is that the synthesis technology for carrying out synthesis of oxalic acid methyl ethyl ester based on micro passage reaction is probed into.Utilize microreactor
The height mixing in channel of slype and feed liquid then reacted, greatly shorten batch tank reactor for a long time
Reaction could obtain the reaction time of preferable yield.
The technical solution adopted in the present invention is as follows:
A method of methyl ethyl oxalate is prepared in micro passage reaction, at least there are two import and one outlets
Reacting for diethy-aceto oxalate and methanol transesterification synthesis of oxalic acid methyl ethyl ester is carried out in micro passage reaction；
Diethy-aceto oxalate and methanol feed liquid is respectively configured, and used catalyst is placed in methanol simultaneously ultrasonic dissolution；It will be careless
Diethyl phthalate and methanol solution pass through high pressure pump respectively and carry out feed liquor, the high pressure infuser can with accuracy controlling feed flow rate,
Solution is infused by high pressure pump pump function and enters the two entrances of micro passage reaction, and flow rates can be
0.001mL/min~10mL/min is adjusted；Micro passage reaction upper substrate is loaded with temperature controlled heating plate, to adjust reaction
Temperature；Pass through the molar ratio of control overall flow rate two solution of constant regulation；Selecting catalyst concentration is dissolved according to catalyst
Mass fraction in methyl alcohol calculates.
In the above method, the solution is not diluted, and two flow velocity adjustable ranges are respectively 5 μ of μ L/min~25 L/
min；(in terms of the residence time)
In the above method, the molar ratio expected range of the methanol and methyl ethyl oxalate is in 1:1~6:1, preferential selection
1.3:1~5:1；
In the above method, the micro passage reaction unit part temperature controlling range is 15 DEG C~60 DEG C, preferential to select
Temperature range is at 20 DEG C~50 DEG C；
In the above method, concentration of the catalyst in methanol solution is 5mg/mL~20mg/mL.
The device of this reaction includes several points:
Two bottles of reaction raw materials liquid via PET pipe conveying respectively enter two high pressure pumps, after through high pressure pump will
Material liquid is pumped into micro passage reaction respectively by PET pipe；
One has the micro passage reaction of temperature control device 13；Including two pieces of stainless steel substrates, i.e. upper substrate 14 and lower base
Plate 9 has three microchannels in lower substrate 9, is two microchannel entrances 5,6 respectively and the microchannel 8 that is attached thereto, and micro- logical
Road 8 is embedded with the capsule shape rubber grain 7 of periodic arrangement above, and two parallel rubber grains are at an angle.To realize two
Stock material is divided into thread to be mixed.
The temperature control device 13 is one to be loaded on the outside of upper substrate 14 and carry out heated for controlling temperature, and be adjusted by liquid crystal display
Temperature；
Reaction solution is reacted in microchannel 8, is discharged to obtain production fluid by channel outlet 10, PET pipe, after by gas phase
Chromatography 12 is detected.
Embodiment 1
Methanol and diethy-aceto oxalate are continuously pumped into microreactor by high pressure pump, and control the temperature at 20 DEG C
Under reacted, control methanol and diethy-aceto oxalate molar ratio 3.3:1, catalyst concn 5mg/mL, pass through control feed liquor
Overall flow rate changes residence time of reaction, residence time of two strands of materials in reactor be respectively 1.38min, 1.73min,
2.3min、3.45min、6.9min。
Production fluid different in flow rate is collected respectively, and is the production fluid for collecting 1h, and product is carried out with gas-chromatography
The conversion ratio of analytical calculation diethy-aceto oxalate, the selectivity and yield of methyl ethyl oxalate, as a result as shown in Fig. 2, in this reality
The flow velocity for applying raising feed liquor under micro passage reaction and reaction condition used is advantageous for the conversion of diethy-aceto oxalate, but for
The selectivity of reaction purpose product is that have a first substantially steady process to decline, this is because being to be flowed in this implementation by changing
Speed changes residence time of reaction, and flow velocity increases the residence time and shortens, and the degree for reacting progress is declined.Preferably stop
Time is 2.3min.
Embodiment 2
Process is same as Example 1, is 2.3min (charging 40 μ L/min of overall flow rate), methanol and oxalic acid two with the residence time
The molar ratio of ethyl ester is 3.3:1, and catalyst concn 5mg/mL, reaction temperature is respectively 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C.With gas
It is as shown in Fig. 3 that phase chromatography carries out analysis reaction result to product.As a result according to the temperature oxalic acid two for shown in attached drawing 3, changing reaction
The conversion ratio variation tendency of ethyl ester is to fall before and have later to remain unchanged slightly, and the conversion ratio of methyl ethyl oxalate and selectivity
There is downward trend in first rising afterwards and obtain peak at 40 DEG C, thus preferably reaction temperature is 40 DEG C.
Embodiment 3
Process is same as Example 1, is 2.3min with the residence time, (charging 40 μ L/min of overall flow rate) reaction temperature is 40
DEG C, the molar ratio of catalyst concn 5mg/mL, methanol and diethy-aceto oxalate are respectively 1.3:1,2:1,3.3:1,5:1.With gas
Phase chromatography analyzes product, the conversion ratio of calculating oxalate diethylester, the selectivity of methyl ethyl oxalate and yield.As a result basis
Attached drawing 4 is it is recognised that be first presented ascendant trend when molar ratio obtains conversion ratio and have in 1.3:1~5:1 diethy-aceto oxalate, and oxalic acid
It is on a declining curve that methyl ethyl ester obtains selectivity, yield variation tendency be first rises decline afterwards and when molar ratio is 2:1 both
It is to obtain maximum value, thus the preferable molar ratio that obtains is 2:1.
Embodiment 4
Process is same as Example 1, is 2.3min with the residence time, (charging 40 μ L/min of overall flow rate) reaction temperature is 40
DEG C, the molar ratio of methanol and oxalate diester is 2:1, and catalyst concn is respectively 5mg/mL, 10mg/mL, 15mg/mL, 20mg/
mL.Product is analyzed with gas-chromatography, the conversion ratio of calculating oxalate diethylester, the selectivity of methyl ethyl oxalate and yield.
As a result with reference to the accompanying drawings 5 it is found that with catalyst concn must increase methyl ethyl oxalate and obtain selectivity and yield be after first increasing under
Drop and obtain maximum value when catalyst concn is 15mg/mL, and diethy-aceto oxalate conversion ratio is then micro- after first reducing
Decline after micro- rising.It is thus preferable that catalyst concn is 15mg/mL.
Embodiment 5
Process is same as Example 1, is 2.3min with the residence time in the case where preferable methyl ethyl oxalate obtains preparation condition, into
Expect 40 μ L/min of overall flow rate) reaction temperature is 40 DEG C, the molar ratio of methanol and oxalate diester is respectively 2:1, and catalyst concn is
15mg/mL.Product is analyzed with gas-chromatography, the conversion ratio of calculating oxalate diethylester, the selectivity of methyl ethyl oxalate and
Yield.As a result with reference to the accompanying drawings 6 it is found that continuously collect 6 production fluids it is recognised that diethy-aceto oxalate obtains conversion ratio, methyl ethyl oxalate
The selectivity and yield amplitude of variation of ethyl ester are smaller, relatively stable.
Claims (10)
1. a kind of system based on micro passage reaction synthesis of oxalic acid methyl ethyl ester, which is characterized in that including the first stock bottle (1),
Second stock bottle (2), micro passage reaction, collection device (11)；
The micro passage reaction includes that first entrance microchannel (5), second entrance microchannel (6), microchannel (8) and channel go out
Mouthful (10), the first entrance microchannel (5) and second entrance microchannel respectively with the first stock bottle (1) and the second stock bottle
(2) it connects, first entrance microchannel (5), second entrance microchannel (6) other end are connect with microchannel (8), the channel outlet
(10) it is connect with collection device (11).
2. system according to claim 1, which is characterized in that first stock bottle (1) and first entrance microchannel (5)
Between connected by the first infusion pump (3), pass through between second stock bottle (2) and second entrance microchannel (6) second defeated
Liquid pump (4) connection.
3. system according to claim 2, which is characterized in that the microchannel (8) is embedded with the glue of periodic arrangement above
Cryptomere rubber grain (7), two parallel rubber grains at an angle, to be divided into thread to mix two strands of materials.
4. system according to claim 3, which is characterized in that the micro passage reaction further includes lower substrate (9), upper base
Plate (14), the first entrance microchannel (5), second entrance microchannel (6), microchannel (8) and channel outlet (10) setting exist
On lower substrate (9).
5. system according to claim 4, which is characterized in that temperature control device (13) are arranged on the upper substrate (14).
6. system according to claim 1, which is characterized in that it further include gas-chromatography (12), the production fluid bottle (11)
Rear end connects gas-chromatography (12).
7. a kind of method using system synthesis methyl ethyl oxalate described in any one of claims 1-6, which is characterized in that including
Following steps:
(1) diethy-aceto oxalate and methanol feed liquid is respectively configured；
(2) diethy-aceto oxalate and methanol solution are passed through into high pressure pump feed liquor respectively, solution is made by high pressure pump pump pressure
The two entrances of micro passage reaction are entered with infusion；It is adjusted by the temperature control device (13) of micro passage reaction upper substrate anti-
Temperature is answered, esterification is carried out；
(3) it is flowed into collection device (11) via channel outlet (10), then methyl ethyl oxalate is detected by gas-chromatography (12)
Yield.
8. the method according to the description of claim 7 is characterized in that passing through the charging of two kinds of materials of control in the step (2)
Flow velocity controls reaction time of the reaction solution in micro passage reaction, catalyst methanol solution flow velocity and diethy-aceto oxalate
Flow velocity be respectively 5 μ L/min of μ L/min~30,5 μ of μ L/min~30 L/min；Reaction temperature is 20 DEG C~50 DEG C.
9. according to the method described in claim 8, it is characterized in that, the overall flow rate is to pass through under 10 μ of μ L/min~60 L/min
Change two bursts of feed flow rates and then change the molar ratio of methanol and diethy-aceto oxalate, molar ratio range is 1.3:1~5:1.
10. according to the method described in claim 8, it is characterized in that, catalyst type in the catalyst methanol be KOH,
K2CO3、KHCO3Or CH3OK, catalyst concn are 5mg/mL~20mg/mL.
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| CN201910557883.9A CN110283071B (en) | 2019-06-26 | 2019-06-26 | System and method for synthesizing ethyl methyl oxalate based on microchannel reactor |
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| CN201910557883.9A CN110283071B (en) | 2019-06-26 | 2019-06-26 | System and method for synthesizing ethyl methyl oxalate based on microchannel reactor |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115106034A (en) * | 2022-06-23 | 2022-09-27 | 之江实验室 | Visual microreactor and preparation method thereof |
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| CN104745310A (en) * | 2015-03-20 | 2015-07-01 | 南京工业大学 | Method for producing biodiesel by adopting microchannel reactor |
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| CN104745310A (en) * | 2015-03-20 | 2015-07-01 | 南京工业大学 | Method for producing biodiesel by adopting microchannel reactor |
Non-Patent Citations (1)
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115106034A (en) * | 2022-06-23 | 2022-09-27 | 之江实验室 | Visual microreactor and preparation method thereof |
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