CN109020811A - The method for preparing propionic ester using microreactor - Google Patents
The method for preparing propionic ester using microreactor Download PDFInfo
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- CN109020811A CN109020811A CN201811091842.7A CN201811091842A CN109020811A CN 109020811 A CN109020811 A CN 109020811A CN 201811091842 A CN201811091842 A CN 201811091842A CN 109020811 A CN109020811 A CN 109020811A
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- microreactor
- metering pump
- blender
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- propionic ester
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- 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
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The invention discloses a kind of methods for preparing propionic ester using microreactor, production equipment includes: that the first, second metering pump is connected to the first blender, third metering pump is connected to the second blender, blender is connected with microreactor, the discharge end of microreactor is provided with the material efferent duct with sampling shut-off valve, material efferent duct is connected to filter, the output end of filter is connected in parallel to drainpipe and drainage conduit, drainage conduit is connected to rectifying column, and the efferent duct of rectifying column is connected with drain sump；Preparation process includes: that propionic acid and monohydric alcohol are pumped by the first, second metering pump respectively, and acidic ionic liquid catalysts are pumped by third metering pump, and at 50 DEG C ~ 100 DEG C, the reaction time is controlled in 5min ~ 60min for reaction temperature control.The invention has the advantages that the speed of material diffusion can be further speeded up, and the uniformity of material mixing is further increased, substantially reduces reaction time and production cycle, low energy consumption, high conversion rate.
Description
Technical field
The present invention relates to the method preparation technical fields of propionic ester, and in particular to prepares propionic ester using microreactor
Method.
Background technique
It is safe and clean, efficient, energy saving and it is sustainable be 21 century development of chemical industry a trend.Microreactor
One is realized the new technology of green syt by process intensification, relative to traditional batch reaction process, is had quickly mixed
Conjunction, efficient heat transfer, narrow residence time destribution, reproducible, system response is rapid, is convenient for automation control, almost without amplification
The advantages such as effect and high safety performance, therefore the research hotspot one of common as research institutions and business circles.Microreactor
It is inside provided with microchannel module, is provided with microchannel in microchannel module.
Propionic ester is important organic compound, can be used as solvent, extractant, fragrance, organic intermediate and plasticizer
Etc..The preparation method of traditional propionic ester is sulfuric acid catalysis esterification process, and sulfuric acid catalysis esterification process is anti-with monohydric alcohol and propionic acid
Raw material is answered, reaction generates propionic ester under conditions of the concentrated sulfuric acid or solid acid or Lewis acid are as catalyst.This method technique at
It is ripe, but have the following deficiencies: that corrosivity is serious, easily causes side reaction, the reaction process three wastes more, it pollutes the environment serious.
For the defect for overcoming traditional preparation methods, my company has developed a kind of propionic ester for using ionic liquid as catalyst
Preparation method, reference can be made to technical solution disclosed in application number 201610591260X.But the preparation method still has following
Defect: the reaction time is long, needs 4~12 hours, and energy consumption is high.
Summary of the invention
The object of the present invention is to provide a kind of reaction time is short, low energy consumption high income, by-product is few, environmental pollution is small
The method for preparing propionic ester using microreactor.
To achieve the above object, the technical solution adopted by the present invention is that: the method for preparing propionic ester using microreactor,
It is characterized by: production equipment includes: the first metering pump, the second metering pump, third metering pump, the first metering pump, the second metering
Pump be connected to the first blender, third metering pump is connected to the second blender, the first blender, the second blender respectively with it is miniature
The feed end of reactor is connected, and the discharge end of microreactor is provided with the material efferent duct with sampling shut-off valve, and material is defeated
Outlet pipe is connected to filter, and the output end of filter is connected with drainpipe and drainage conduit, and drainage conduit is connected to rectifying column, rectifying column
Efferent duct be connected with drain sump；Reaction raw materials include: propionic acid, monohydric alcohol, acidic ionic liquid catalysts, propionic acid and unitary
The molar ratio of alcohol is controlled in 1:(1.0 ~ 5.0), the dosage of acidic ionic liquid catalysts be reaction raw materials gross mass 0.1% ~
1%；Preparation process includes: that propionic acid and monohydric alcohol are pumped by the first metering pump, the second metering pump respectively, presence of acidic ionic liquid catalyst
Agent is pumped by third metering pump, and the reaction raw materials in the first blender and the second blender enter in microreactor, reaction
Temperature control is at 50 DEG C ~ 100 DEG C, and reaction time control is in 5min ~ 60min, the object of the material efferent duct output of microreactor
Material, which enters to, filters layering in filter, wherein organic layer enters rectifying in rectifying column and obtains crude product, and crude product enters in drain sump
Finished product is obtained after dehydration.
Further, the method above-mentioned for preparing propionic ester using microreactor, wherein the draining of filter output end
Pipe is connected with water recovery tank, and the water layer that filtering layering obtains in filter is entered in water recovery tank by drainpipe.
Further, the method above-mentioned for preparing propionic ester using microreactor, wherein be connected at the top of rectifying column
Rectifying drainpipe, rectifying drainpipe are connected with water recovery tank.
Further, the method above-mentioned for preparing propionic ester using microreactor, wherein in the shell of microreactor
It is provided with ultrasonic transducer, ultrasonic transducer is located at outside the tube wall of the microchannel in microreactor, ultrasonic transducer
The tube wall of microchannel can be made to generate vibration.
Further, the method above-mentioned for preparing propionic ester using microreactor, wherein band valve is provided on drain sump
Drain sump efferent duct, drain sump efferent duct is connected with finished pot, and the finished product that formation is dehydrated in drain sump is defeated by drain sump
Outlet pipe enters in finished pot.
Further, the method above-mentioned for preparing propionic ester using microreactor, wherein microreactor temperature control reaction
After a period of time, from the sampling end sampling monitoring of sampling valve shut-off valve, when alcohol content is less than 1%, determines that reaction terminates, open
Shut-off valve is sampled, the material after reacting in microreactor is allowed to enter in filter from material efferent duct.
Further, the method above-mentioned for preparing propionic ester using microreactor, wherein the monohydric alcohol of reaction raw materials is
One of methanol, ethyl alcohol, propyl alcohol, butanol.
Further, the method above-mentioned for preparing propionic ester using microreactor, wherein in reaction raw materials it is acid from
Sub- liquid catalyst is double fluorine sulfimide imidazole salts.
Further, the method above-mentioned for preparing propionic ester using microreactor, wherein micro- logical in microreactor
The diameter in road is the mm of 0.1 mm ~ 2.0, and length is the m of 20 m ~ 50.
The invention has the advantages that the uniformity of one, reaction raw materials mixing greatly improves, reaction raw materials contact is more abundant,
Compared to traditional production technology, reaction time and production cycle are substantially reduced.Two, the caliber of microreactor channels it is small,
Large specific surface area, it is safe and efficient, there is good mass transfer effect, material can quickly come into full contact with reaction with precise proportions, temperature
Degree control is accurate, and low energy consumption, and high conversion rate can be continuously produced, and the generation of by-product is effectively reduced, to greatly improve mole
Yield.Three, ultrasonic transducer is set in the shell of microreactor, the speed of material diffusion can be further speeded up, gone forward side by side
One step improves the uniformity of material mixing, to further increase reaction efficiency.Four, entire reaction system has without enlarge-effect
Conducive to industrial application.
Detailed description of the invention
Fig. 1 is the arrangement of the present invention that production equipment used in the method for propionic ester is prepared using microreactor
Structural schematic diagram.
Specific embodiment
It elaborates below to the method for preparing propionic ester using microreactor.
As shown in Figure 1, the method for preparing propionic ester using microreactor, the production equipment of use includes: the first metering
The 1, second metering pump 2, third metering pump 3 are pumped, the first metering pump 1, the second metering pump 2 are connected to the first blender 4, third metering
Pump 3 is connected to the second blender 5, and the first blender 4, the second blender 5 are connected with the feed end of microreactor 7 respectively.
The diameter of microchannel in microreactor 7 is preferably the mm of 0.1 mm ~ 2.0, and length is preferably the m of 20 m ~ 50.The present embodiment
In, to improve the uniformity that material mixes, ultrasonic transducer, ultrasonic transducer are provided in the shell of microreactor 7
Outside the tube wall of microchannel in microreactor, ultrasonic transducer can make the tube wall of microchannel generate vibration, thus
The uniformity for further increasing material dispersion keeps material diffusion more quickly abundant, further increases reaction efficiency.Minisize reaction
The discharge end of device 7 is provided with the material efferent duct 8 with sampling shut-off valve 81, and material efferent duct 8 is connected to filter 9, filter 9
Output end be connected with drainpipe 10 and drainage conduit 11, drainpipe 10 is connected with water recovery tank 6, in filter 9 filter layering
Obtained water layer is entered in water recovery tank 6 by drainpipe 10.Drainage conduit 11 is connected to rectifying column 12, the output of rectifying column 12
Pipe is connected with drain sump 13, and the top of rectifying column 12 is connected with rectifying drainpipe 121, rectifying drainpipe 121 and water recovery tank 6
It is connected, the moisture that when rectifying generates enters in water recovery tank 6 from rectifying drainpipe 121.Band valve is provided on drain sump 13
Drain sump efferent duct 131, drain sump efferent duct 131 is connected with finished pot 14.
Reaction raw materials include: propionic acid, monohydric alcohol, acidic ionic liquid catalysts.The control of the molar ratio of propionic acid and monohydric alcohol
In 1:(1.0 ~ 5.0), the dosage of acidic ionic liquid catalysts is the 0.1% ~ 1% of reaction raw materials gross mass.The monohydric alcohol
For one of methanol, ethyl alcohol, propyl alcohol, butanol.The acidic ionic liquid catalysts are double fluorine sulfimide imidazole salts.
Preparation process includes: that propionic acid and monohydric alcohol are pumped by the first metering pump 1, the second metering pump 2 respectively, acidic ionic liquid
Body catalyst is pumped by third metering pump 3, and the reaction raw materials in the first blender 4 and the second blender 5 enter to minisize reaction
In device 7, at 50 DEG C ~ 100 DEG C, the reaction time is controlled in 5min ~ 60min for reaction temperature control.: the reaction of 7 temperature control of microreactor
After a period of time, from the sampling end sampling monitoring of sampling shut-off valve 81, when alcohol content is less than or equal to 1%, determine that reaction terminates,
Sampling shut-off valve 81 is opened, the material after reacting in microreactor 7 is allowed to enter in filter 9 from material efferent duct 8.It is miniature
The material that the material efferent duct 8 of reactor 7 exports, which enters to, filters layering in filter 9, wherein organic layer enters rectifying column 12
In, 12 rectifying of rectifying column obtains crude product, and crude product, which enters to, obtains finished product after dehydration in drain sump 13.In drain sump 13 dehydration formed at
Product are entered in finished pot 14 by drain sump efferent duct 131.
It is further described in detail to be done to the method for preparing propionic ester using microreactor, specific reality is given below
Apply example.
Embodiment 1.
Reaction raw materials: propionic acid 74g(1mol), 38.4 g(1.2mol of methanol), acidic ionic liquid catalysts --- double fluorine
Sulfimide imidazole salts 0.22g(accounts for the 0.2% of reaction raw materials gross mass).
Propionic acid and methanol are passed through into the first metering pump 1 respectively and the second metering pump 2 is pumped into the first blender 4, double fluorine sulphurs
Acid imide imidazole salts are pumped into the second blender 5 by third metering pump 3.Liquid in first blender 4 and the second blender 5
Into in microreactor 7,50 DEG C of temperature control 10 min of reaction, from the sampling end sampling monitoring of sampling shut-off valve 81, alcohol content is
0.02%, judge that reaction terminates.Sampling shut-off valve 81 is opened, the material in microreactor 7 was entered by material efferent duct 8
In filter 9, water-yielding stratum and organic layer are separated in filter 9, water layer is entered in water recovery tank 6 by drainpipe 10, organic layer
Enter rectifying in rectifying column 12 by drainage conduit 11, a small amount of moisture that 12 rectifying of rectifying column generates enters through rectifying drainpipe 121
Into water recovery tank 6,80 DEG C of the fraction containing micro-moisture --- crude product is collected in 12 rectifying of rectifying column, and crude product enters drain sump 13
In slough micro-moisture, obtain finished product 85.62g(purity 99.91%, molar yield: 97.1%) finished product is transferred in finished pot 14.
Embodiment 2.
Reaction raw materials: propionic acid 74g(1mol), ethyl alcohol 69.10g(1.5mol), acidic ionic liquid catalysts --- double fluorine
Sulfimide imidazole salts 0.36g(accounts for the 0.25% of reaction raw materials gross mass).
Propionic acid and ethyl alcohol are passed through into the first metering pump 1 respectively and the second metering pump 2 is pumped into the first blender 4, double fluorine sulphurs
Acid imide imidazole salts are pumped into the second blender 5 by third metering pump 3.Liquid in first blender 4 and the second blender 5
Into in microreactor 7,60 DEG C of temperature control 40 min of reaction, from the sampling end sampling monitoring of sampling shut-off valve 81, alcohol content is
0.04%, judge that reaction terminates.Sampling shut-off valve 81 is opened, the material in microreactor 7 was entered by material efferent duct 8
In filter 9, water-yielding stratum and organic layer are separated in filter 9, water layer is entered in water recovery tank 6 by drainpipe 10, organic layer
Enter rectifying in rectifying column 12 by drainage conduit 11, a small amount of moisture that 12 rectifying of rectifying column generates enters through rectifying drainpipe 121
Into water recovery tank 6,80 DEG C of the fraction containing micro-moisture --- crude product is collected in 12 rectifying of rectifying column, and crude product enters drain sump 13
In slough micro-moisture, obtain finished product 99.08g(purity 99.89%, molar yield: 96.91%) finished product is transferred in finished pot 14.
Embodiment 3.
Reaction raw materials: propionic acid 74g(1mol), propyl alcohol 78g(1.3mol), acidic ionic liquid catalysts --- double fluorine sulphonyl
Imine imidazole salt 0.46g(accounts for the 0.3% of reaction raw materials gross mass).
Propionic acid and propyl alcohol are passed through into the first metering pump 1 respectively and the second metering pump 2 is pumped into the first blender 4, double fluorine sulphurs
Acid imide imidazole salts are pumped into the second blender 5 by third metering pump 3.Liquid in first blender 4 and the second blender 5
Into in microreactor 7,55 DEG C of temperature control 60 min of reaction, from the sampling end sampling monitoring of sampling shut-off valve 81, alcohol content is
0.03%, judge that reaction terminates.Sampling shut-off valve 81 is opened, the material in microreactor 7 was entered by material efferent duct 8
In filter 9, water-yielding stratum and organic layer are separated in filter 9, water layer is entered in water recovery tank 6 by drainpipe 10, organic layer
Enter rectifying in rectifying column 12 by drainage conduit 11, a small amount of moisture that 12 rectifying of rectifying column generates enters through rectifying drainpipe 121
Into water recovery tank 6,80 DEG C of the fraction containing micro-moisture --- crude product is collected in 12 rectifying of rectifying column, and crude product enters drain sump 13
In slough micro-moisture, obtain finished product 112.87g(purity 99.86%, molar yield: 97.03%) finished product is transferred in finished pot 14.
Embodiment 4.
Reaction raw materials: propionic acid 74g(1mol), ethyl alcohol 92.14g(2.0mol), acidic ionic liquid catalysts --- double fluorine
Sulfimide imidazole salts 0.66g(accounts for the 0.4% of reaction raw materials gross mass).
Propionic acid and ethyl alcohol are passed through into the first metering pump 1 respectively and the second metering pump 2 is pumped into the first blender 4, double fluorine sulphurs
Acid imide imidazole salts are pumped into the second blender 5 by third metering pump 3.Liquid in first blender 4 and the second blender 5
Into in microreactor 7,55 DEG C of temperature control 60 min of reaction, from the sampling end sampling monitoring of sampling shut-off valve 81, alcohol content is
0.05%, judge that reaction terminates.Sampling shut-off valve 81 is opened, the material in microreactor 7 was entered by material efferent duct 8
In filter 9, water-yielding stratum and organic layer are separated in filter 9, water layer is entered in water recovery tank 6 by drainpipe 10, organic layer
Enter rectifying in rectifying column 12 by drainage conduit 11, a small amount of moisture that 12 rectifying of rectifying column generates enters through rectifying drainpipe 121
Into water recovery tank 6,80 DEG C of the fraction containing micro-moisture --- crude product is collected in 12 rectifying of rectifying column, and crude product enters drain sump 13
In slough micro-moisture, obtain finished product 99.54g(purity 99.85%, molar yield: 97.32%) finished product is transferred in finished pot 14.
Embodiment 5.
Reaction raw materials: propionic acid 74g(1mol), propyl alcohol 84.10g(1.4mol), acidic ionic liquid catalysts --- double fluorine
Sulfimide imidazole salts 0.24g(accounts for the 0.15% of reaction raw materials gross mass).
Propionic acid and ethyl alcohol are passed through into the first metering pump 1 respectively and the second metering pump 2 is pumped into the first blender 4, double fluorine sulphurs
Acid imide imidazole salts are pumped into the second blender 5 by third metering pump 3.Liquid in first blender 4 and the second blender 5
Into in microreactor 7,100 DEG C of temperature control 5 min of reaction, from the sampling end sampling monitoring of sampling shut-off valve 81, alcohol content is
0.08%, judge that reaction terminates.Sampling shut-off valve 81 is opened, the material in microreactor 7 was entered by material efferent duct 8
In filter 9, water-yielding stratum and organic layer are separated in filter 9, water layer is entered in water recovery tank 6 by drainpipe 10, organic layer
Enter rectifying in rectifying column 12 by drainage conduit 11, a small amount of moisture that 12 rectifying of rectifying column generates enters through rectifying drainpipe 121
Into water recovery tank 6,80 DEG C of the fraction containing micro-moisture --- crude product is collected in 12 rectifying of rectifying column, and crude product enters drain sump 13
In slough micro-moisture, obtain finished product 113.13g(purity 99.88%, molar yield: 97.28%) finished product is transferred in finished pot 14.
The invention has the advantages that the uniformity of one, reaction raw materials mixing greatly improves, reaction raw materials contact is more abundant,
Compared to traditional production technology, reaction time and production cycle are substantially reduced.Two, the caliber of microreactor channels it is small,
Large specific surface area, it is safe and efficient, there is good mass transfer effect, material can quickly come into full contact with reaction with precise proportions, temperature
Degree control is accurate, and low energy consumption, and high conversion rate can be continuously produced, and the generation of by-product is effectively reduced, to greatly improve mole
Yield.Three, ultrasonic transducer is set in the shell of microreactor, the speed of material diffusion can be further speeded up, gone forward side by side
One step improves the uniformity of material mixing, to further increase reaction efficiency.Four, entire reaction system has without enlarge-effect
Conducive to industrial application.
Claims (9)
1. the method for preparing propionic ester using microreactor, it is characterised in that: production equipment includes: the first metering pump, second
Metering pump, third metering pump, the first metering pump, the second metering pump are connected to the first blender, and third metering pump is blended with second
Device connection, the first blender, the second blender are connected with the feed end of microreactor respectively, the discharge end of microreactor
It is provided with the material efferent duct with sampling shut-off valve, material efferent duct is connected to filter, and the output end of filter is connected with row
Water pipe and drainage conduit, drainage conduit are connected to rectifying column, and the efferent duct of rectifying column is connected with drain sump；Reaction raw materials include: third
The molar ratio of acid, monohydric alcohol, acidic ionic liquid catalysts, propionic acid and monohydric alcohol is controlled in 1:(1.0 ~ 5.0), acidic ionic liquid
The dosage of body catalyst is the 0.1% ~ 1% of reaction raw materials gross mass；Preparation process includes: propionic acid and monohydric alcohol respectively by the first meter
Amount pump, the pumping of the second metering pump, acidic ionic liquid catalysts are pumped by third metering pump, the first blender and the second blender
In reaction raw materials enter in microreactor, reaction temperature control at 50 DEG C ~ 100 DEG C, reaction time control 5min ~
60min, the material of the material efferent duct output of microreactor, which enters to, filters layering in filter, wherein organic layer enters essence
It evaporates rectifying in tower and obtains crude product, crude product, which enters to, obtains finished product after dehydration in drain sump.
2. the method according to claim 1 for preparing propionic ester using microreactor, it is characterised in that: filter output
The drainpipe at end is connected with water recovery tank, and the water layer that filtering layering obtains in filter enters to water recovery tank by drainpipe
In.
3. the method according to claim 2 for preparing propionic ester using microreactor, it is characterised in that: the top of rectifying column
Portion is connected with rectifying drainpipe, and rectifying drainpipe is connected with water recovery tank.
4. the method according to claim 1 for preparing propionic ester using microreactor, it is characterised in that: microreactor
Shell in be provided with ultrasonic transducer, ultrasonic transducer is located at outside the tube wall of the microchannel in microreactor, ultrasound
Wave transducer can make the tube wall of microchannel generate vibration.
5. the method according to claim 1 for preparing propionic ester using microreactor, it is characterised in that: set on drain sump
It is equipped with the drain sump efferent duct with valve, drain sump efferent duct is connected with finished pot, and the finished product that formation is dehydrated in drain sump passes through
Drain sump efferent duct enters in finished pot.
6. the method for preparing propionic ester using microreactor described according to claim 1 or 2 or 3 or 4 or 5, feature exist
In: after microreactor temperature control reacts a period of time, from the sampling end sampling monitoring of sampling valve shut-off valve, when alcohol content is less than 1%
When, determine that reaction terminates, opens sampling shut-off valve, the material after reacting in microreactor is allowed to enter to from material efferent duct
In filter.
7. the method for preparing propionic ester using microreactor described according to claim 1 or 2 or 3 or 4 or 5, feature exist
In: the monohydric alcohol of reaction raw materials is one of methanol, ethyl alcohol, propyl alcohol, butanol.
8. the method for preparing propionic ester using microreactor described according to claim 1 or 2 or 3 or 4 or 5, feature exist
In: the acidic ionic liquid catalysts in reaction raw materials are double fluorine sulfimide imidazole salts.
9. the method for preparing propionic ester using micro passage reaction described according to claim 1 or 2 or 3 or 4 or 5, feature
Be: the diameter of the microchannel in microreactor is the mm of 0.1 mm ~ 2.0, and length is the m of 20 m ~ 50.
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| CN111302937A (en) * | 2020-04-08 | 2020-06-19 | 北京理工大学 | Method for preparing p-tert-butyl methyl benzoate |
| CN114773241A (en) * | 2022-04-20 | 2022-07-22 | 益丰新材料股份有限公司 | Continuous synthesis method of mercaptocarboxylic ester |
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