CN208894182U - A kind of continuous flow catalytic reactor - Google Patents
A kind of continuous flow catalytic reactor Download PDFInfo
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- CN208894182U CN208894182U CN201821602001.3U CN201821602001U CN208894182U CN 208894182 U CN208894182 U CN 208894182U CN 201821602001 U CN201821602001 U CN 201821602001U CN 208894182 U CN208894182 U CN 208894182U
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- continuous flow
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Abstract
The utility model discloses a kind of continuous flow catalytic reactors.The continuous flow catalytic reactor includes reaction vessel, the filler being packaged in the reaction vessel and electrically charged catalyst component, and the catalyst component is fixed on the filler under DC electric field effect.The continuous flow catalytic reactor can be applied to the reaction of the continuous flows such as monosaccharide epimerization reaction.The continuous flow catalytic reactor of the utility model have structure it is simple, can be unattended, the advantages such as easy-to-operate, and during being applied to continuous flow reaction, since catalyst component is fixed by direct current place, it will not be flowed out with product, the separating step for saving catalyst improves the utilization efficiency of catalyst.
Description
Technical field
The utility model is specifically related to a kind of continuous flow catalytic reactor, its assemble method and application, such as poor in monosaccharide
Application into isomerization reaction.
Background technique
Traditional autoclave liquid phase reactor solves the problems, such as a large amount of chemical products demands, but there is also much itself be difficult to overcome
The shortcomings that, such as security risk, environmental pollution, energy consumption be huge, unstable product quality, takes up a large area and technique amplification
Difficulty etc. (chemical progress, 2016,28 (6): 829-838).Continuous flow reaction is passed with its unique hybrid mode, efficient mass transfer
Hot, low solvent acquisition solves these problems just." continuous flow chemistry " or it is " flowing chemistry ", refers to and object is conveyed by pump
The technology expected and chemically reacted with continuous flow modes.In the past 20 years, continuous flow reaction technology is in academia and industry
More and more welcomed by the people, its advantage is mainly reflected in: (1) reactor size is small, and mass-and heat-transfer is rapid, easily realizes
Cheng Qianghua；(2) state modulator is accurate, good reaction selectivity, is particularly suitable for inhibiting series connection side reaction；(3) online inventory is few,
The intrinsic flame retardant property of minim channel, small structure enhancement device explosion-proof performance, safe operation；(4) continuous operation, spatiotemporal efficiency
It is high；(5) automation control easy to accomplish, enhances the safety of operation, save human resources (Chinese Journal of Pharmaceuticals,
2017,48 (4): 469-482).
The continuous flow reaction of liquid phase is mostly catalysis reaction, will generally be passed through after catalyst and raw material premix reactor carry out it is anti-
It answers.If catalyst is fixed in the reactor, catalyst separating step can be saved, the loss of catalyst is reduced, promotes it
Utilization efficiency prolongs its service life.Common catalyst fixing means is physisorphtion and chemical bonding method.
CN101033192A discloses a kind of continuous flow reaction method of preparing nitrobenzene from benzene by nitric acid nitrating, by impregnating metal oxygen
Compound loads on MFI topological structure molecular sieve and boehmite, and the type that is then pressed into is fixed bed catalyst；
Biggelaar etc. is by covalent bond by ω-transaminase by being fixed on the modified porous oxidation of 3- aminopropyl triethoxysilane
On silicon, the continuous flow for enantioselectivity transamination reacts (Catalysts, 2017,7 (54): 1-13)；Deng
Molybdenum acid ion is fixed on anion exchange resin using ionic bond, the epimerization for glucose to mannose is anti-
Answer (Applied Catalysis A, 2008,334 (1-2): 112-118).Although from this way, catalytic active component and carrier knot
It is limited with joint efforts, continuous flow reaction in readily soluble feed liquor phase medium and lose activity, cause catalyst life limited.
Utility model content
The main purpose of the utility model is to provide a kind of continuous flow catalytic reactors, to overcome in the prior art
It is insufficient.
For realization foregoing purpose, the technical solution adopted in the utility model includes:
The utility model embodiment provides a kind of continuous flow catalytic reactor, including reaction vessel and is packaged in described
Filler in reaction vessel；It is characterized by: the continuous flow catalytic reactor further includes electrically charged catalyst component, it is described to urge
Change component to be fixed on the filler under DC electric field effect.
In some embodiments, the reaction vessel is tubular structure.
In some embodiments, the reaction vessel is glass material.
In some embodiments, the filler includes active carbon, any one or two kinds in ion exchange resin
Combination.
In some embodiments, the catalyst component includes quantum dot, such as can be molybdenum oxide quantum dot.
In some embodiments, the catalyst component includes molybdenum acid ion, ferric hydroxide colloid particle, but is not limited to
This.
Compared with the prior art, the continuous flow catalytic reactor of the utility model have structure it is simple, can be unattended, operation
Electrically charged catalyst component is fixed on filler by the advantages such as safe ready using DC electric field, constitutes fixed bed catalyst.?
Reaction solution is inputted under target temperature, is reacted under the action of catalyst component, and then be continuously available target product.It crosses herein
Cheng Zhong will not be flowed out since catalyst component is fixed by direct current place with product, save the separating step of catalyst, be promoted
The utilization efficiency of catalyst.Using the reactor, it can use molybdenum oxide quantum dot or molybdenum acid ion etc. and be used as catalysis group
Point, realize the successive reaction of monosaccharide epimerization.In addition, applying direct current electric field may promote the change of certain pairs of electric field-sensitives
Learn reaction.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of continuous flow catalytic reactor in the utility model embodiment 1.
Specific embodiment
In view of the deficiencies in the prior art, inventor is studied for a long period of time and is practiced, and is able to propose the skill of the utility model
Art scheme will illustrate in more detail as follows.
A kind of continuous flow catalytic reactor provided by the embodiment of the utility model, including reaction vessel, be packaged in it is described anti-
The filler and electrically charged catalyst component in container are answered, the catalyst component is fixed in described fill out under DC electric field effect
On material.
In some embodiments, the reaction vessel is tubular structure.
In some embodiments, the reaction vessel is glass material, naturally it is also possible to be other materials, such as make pottery
Porcelain material, organic material, etc..
In some embodiments, the filler includes active carbon, any one or two kinds in ion exchange resin
Combination, and it is without being limited thereto.
In some embodiments, the catalyst component includes quantum dot, such as can be molybdenum oxide quantum dot.
In some embodiments, the catalyst component includes molybdenum acid ion, ferric hydroxide colloid particle, but is not limited to
This.
In some embodiments, the internal diameter of the reaction vessel is 1.5~2 centimetres, and length is 50~80 centimetres, volume
It is 100-200 milliliters.
In some embodiments, the particle size of the filler be 10~50 mesh, and the gross mass of the filler with
The mass volume ratio of the volume of the reaction vessel is 50~120 grams: 100~200 milliliters.
In some embodiments, the voltage for being used to form the DC power supply of the DC electric field is 5~50 volts.
The utility model embodiment additionally provides the assemble method of aforementioned any continuous flow catalytic reactor comprising:
Filler is packed into reaction vessel, and by the liquid flow inlet of reaction vessel and fluid outlet with fiber plug envelope
Stifled, the fiber plug can be such that liquid stream passes through but stop the filler；
The liquid flow inlet of the reaction vessel, fluid outlet are electrically connected with the positive or negative pole of DC power supply, and by institute
The cathode or anode for stating DC power supply are connect with the middle section of the filler；
By the solution comprising electrically charged catalyst component from after liquid flow inlet input reaction vessel, then by the liquid stream
Outlet output, so that the catalyst component be made to be fixed on the filler.
In some embodiments, the fiber plug includes mineral wool or silica wool etc., but not limited to this.
In some more specific embodiments, filler can be packed into reaction tube, both ends mineral wool or silica wool envelope
Stifled, filler middle section is shorted DC power anode or cathode, and both ends mineral wool or silica wool are shorted opposite electrode, after energization,
Aqueous solution by certain volume containing catalyst component is pumped into from reaction tube one end, and the other end pumps out.
In some embodiments, the voltage of the DC power supply is 5~50 volts.
In some embodiments, the solution comprising electrically charged catalyst component is quantum dot solution.
In some embodiments, the concentration of the quantum dot solution be 0.5~1 grams per liter, flow be 0.2~1 milliliter/
Minute.
In some embodiments, the solution comprising electrically charged catalyst component is to contain ferric hydroxide colloid particle
Or the solution of molybdenum acid ion.
It is anti-in monosaccharide epimerization that the utility model embodiment additionally provides aforementioned any continuous flow catalytic reactor
Application in answering.The utility model embodiment additionally provides a kind of monosaccharide epimerization reaction method comprising:
Any continuous flow catalytic reactor above-mentioned is provided；
The continuous flow catalytic reactor is electrically connected with DC power supply, to form the DC electric field；And
Reaction vessel is heated to target temperature, and monosaccharide solutions are inputted from the liquid flow inlet of the reaction vessel, then
It include the solution of target product from the collection of the fluid outlet of the reaction vessel.
In some embodiments, the target temperature is 60~120 DEG C.
In some embodiments, the voltage of the DC power supply is 5~50 volts.
In some embodiments, the monosaccharide solutions include glucose, mannose, arabinose, ribose, xylose and come
The combination of any one or more in threose, and it is without being limited thereto.
In some embodiments, the concentration of the monosaccharide solutions is 1~10wt%.
In some embodiments, the flow of the monosaccharide solutions is 0.1~2 ml/min.
In continuous flow catalytic reactor provided by the utility model, electrically charged catalyst component is fixed using DC electric field
On filler, fixed bed catalyst is constituted, so as to inhibit its loss in continuous flow reaction well.
The continuous flow catalytic reactor of the utility model have structure it is simple, can be unattended, easy-to-operate etc. is excellent
Gesture.Using the continuous flow catalytic reactor of the utility model, a variety of continuous flow reactions can be carried out, for example, can be with oxidation
Molybdenum quantum dot or molybdic acid ion etc. are catalyst component, realize the successive reaction of monosaccharide epimerization.In continuous flow reaction process
In, it is pumped into reaction solution under target temperature, is reacted with catalyst component effect, to be continuously available target product.Wherein,
It since catalyst component is fixed by direct current place, will not be flowed out with product, save the separating step of catalyst, improve catalysis
The utilization efficiency of agent.
The utility model is described in detail below in conjunction with reference to the accompanying drawings and examples.It should be noted that not
In the case where conflict, the features in the embodiments and the embodiments of the present application be can be combined with each other.
Embodiment 1: a kind of structure of continuous flow catalytic reactor of the present embodiment is as shown in Figure 1.Wherein, reaction tube 1 is w
Type, glass material, 1.8 centimetres of internal diameter, 70 centimetres of length, 178 milliliters of volume.The coconut activated carbon filling material 2 of filling in reaction tube 1,
12~30 mesh of partial size, 80 grams of quality, filler both ends use silica wool 3,4 to encapsulate respectively；Near inlet 5 and liquid outlet 6 respectively
Opening 7,8 seals fixed graphite electrode 11,12 with silica gel plug 9,10；Two electrodes go deep into reaction tube 1 and silica wool 3,4 is shorted,
And it is shorted with 13 cathode of DC power supply；The opening 14 in reaction tube middle position seals fixed graphite electrode 16, electricity with silica gel plug 15
It is profound enter reaction tube 1 and filler 2 be shorted, and be shorted with 13 anode of DC power supply.
Prepare 200 milliliters of molybdenum oxide quantum dot solutions, concentration is 0.8 grams per liter.DC power supply 13 is opened, voltage is maintained at
24 volts, solution is pumped into reaction tube 1 from inlet with the flow of 0.5 ml/min, flows through filler 2, pumps out from liquid outlet 6,
For quantum dot by Electro Sorb on filler 2, solution obtains continuous flow catalytic reactor after all flowing out.
Embodiment 2: chloride ion exchanger resin filler 2,20~50 mesh of partial size, matter are filled in the reaction tube 1 described in embodiment 1
100 grams of amount, filler both ends use mineral wool 3,4 to encapsulate respectively, with DC power supply connection type with embodiment 1.
Prepare 400 milliliters of molybdenum acid solutions, 0.2 grams per liter of concentration.DC power supply 13 is opened, voltage is maintained at 10 volts, solution
It is pumped into reaction tube 1 from inlet with the flow of 2 ml/mins, flows through filler 2, is pumped out from liquid outlet 6, molybdic acid ion is electric
It is adsorbed on filler 2, obtains continuous flow catalytic reactor.
Embodiment 3: coconut activated carbon filling material 2,12~30 mesh of partial size, quality 80 are filled in the reaction tube 1 described in embodiment 1
Gram.Mineral wool 3,4 is used to encapsulate respectively in filler both ends.DC power supply positive and negative anodes connect direction and embodiment 1 on the contrary, filler both ends
Mineral wool 3,4 is shorted 13 anode of power supply, and middle section is shorted 14 cathode of power supply.
Prepare 100 milliliters of ferric hydroxide sols, 2 grams per liter of concentration.Open DC power supply 13, voltage is maintained at 50 volts, molten
Glue is pumped into reaction tube 1 from inlet with the flow of 0.2 ml/min, flows through filler 2, pumps out from liquid outlet 6, iron hydroxide
Colloidal particle on filler 2, obtains continuous flow catalytic reactor by Electro Sorb.
Embodiment 4: it is heated, reaction tube 1 is immersed in water-bath, feed liquor using reactor of the water-bath mode to embodiment 1
Mouth 5 and liquid outlet 6 are maintained at the water surface or more, are heated to 80 DEG C, open DC power supply 13, voltage maintains 24 volts；From feed liquor
Mouth 5 is pumped into glucose solution, and the mass concentration of glucose solution is 3%, and flow is 0.3 ml/min；It is collected from liquid outlet 6
The solution of the mannose containing target product.Successive reaction 7 days, the yield of mannose maintained 23% or so.
Embodiment 5: it is heated, reaction tube 1 is immersed in oil bath pan, feed liquor using reactor of the oil bath mode to embodiment 1
Mouth 5 and liquid outlet 6 are maintained at pasta or more, are heated to 90 DEG C, open DC power supply 13, voltage maintains 24 volts；From feed liquor
Mouth 5 is pumped into mannose sugar juice, and the mass concentration of mannose solution is 1%, and flow is 0.1 ml/min；It is received from liquid outlet 6
Collect the solution of the glucose containing target product.Successive reaction 7 days, the yield of glucose maintained 60% or so.
Embodiment 6: it is heated, reaction tube 1 is immersed in oil bath pan, feed liquor using reactor of the oil bath mode to embodiment 2
Mouth 5 and liquid outlet 6 are maintained at pasta or more, are heated to 100 DEG C, open DC power supply 13, voltage maintains 40 volts；From feed liquor
Mouth 5 is pumped into arabinose solution, and the mass concentration of arabinose solution is 5%, and flow is 1 ml/min；It is received from liquid outlet 6
Collect the solution of the ribose containing target product.Successive reaction 3 days, the yield of ribose maintained 35% or so.
Embodiment 7: it is heated, reaction tube 1 is immersed in oil bath pan, feed liquor using reactor of the oil bath mode to embodiment 2
Mouth 5 and liquid outlet 6 are maintained at the water surface or more, are heated to 100 DEG C, open DC power supply 13, voltage maintains 40 volts；From feed liquor
Mouth 5 is pumped into ribose solution, and the mass concentration of ribose solution is 5%, and flow is 1 ml/min；It is collected from liquid outlet 6 and contains target
The solution of products arabinose.Successive reaction 3 days, the yield of arabinose maintained 62% or so.
Embodiment 8: it is heated, reaction tube 1 is immersed in oil bath pan, feed liquor using reactor of the oil bath mode to embodiment 1
Mouth 5 and liquid outlet 6 are maintained at pasta or more, are heated to 110 DEG C, open DC power supply 13, voltage maintains 10 volts；From feed liquor
Mouth 5 is pumped into xylose solution, and the mass concentration of xylose solution is 10%, and flow is 2 ml/mins；It is collected from liquid outlet 6 and contains target
The solution of product lyxose.Successive reaction 3 days, the yield of lyxose maintained 30% or so.
Embodiment 9: it is heated, reaction tube 1 is immersed in oil bath pan, feed liquor using reactor of the oil bath mode to embodiment 1
Mouth 5 and liquid outlet 6 are maintained at pasta or more, are heated to 120 DEG C, open DC power supply 13, voltage maintains 10 volts；From feed liquor
Mouth 5 is pumped into lysol sugar juice, and the mass concentration of lysol sugar juice is 10%, and flow is 2 ml/mins；Contain from the collection of liquid outlet 6
The solution of target product xylose.Successive reaction 3 days, the yield of xylose maintained 52% or so.
1:250 grams of sodium molybdate of comparative example is dissolved in water, is settled to 500 milliliters, and 303 grams of chloride ion exchanger resins, room temperature is added
Stirring 16 hours is added 5 33% hydrogen peroxide solutions of drop, was washed with water filter solid 5 times, the hydrochloric acid of 1 mol/L is added dropwise after blotting
PH=3.5 is adjusted, moist catalysis is obtained by filtration.By moist catalysis be fitted into 25 milliliters can electric heating tool thermocouple glass tube in,
It is encapsulated at melten glass with mineral wool, obtains continuous flow reactor.Glucose is pumped into 50 mls/hour of flow at 90 DEG C
Solution (hydrochloric acid of mass concentration 50%, 1 mol/L adjusts pH=3.5) carries out the reaction of epimerization continuous flow.Mannose
Initial yield is 22% or so, and since molybdenum is lost, after reaction 3 days, yield is down to 3%.(bibliography: Applied
Catalysis A, 2008,334 (1-2): 112-118).
70 DEG C of 2:44.14 grams of molybdic acid of comparative example is dissolved in water, is settled to 500 milliliters, is added 50 grams of chloride ion exchanger resins, and 40
DEG C stirring 24 hours, be added dropwise 1 mol/L hydrochloric acid adjust pH=3.5, be then washed with water filter solid 5 times, and obtained wet catalysis
Agent.By moist catalysis be fitted into 25 milliliters can electric heating tool thermocouple glass tube in, encapsulated, obtained with mineral wool at melten glass
To continuous flow reactor.Glucose solution (mass concentration 50%, 1 mol/L are pumped into 50 mls/hour of flow at 90 DEG C
Hydrochloric acid adjust pH=3.5) carry out the reaction of epimerization continuous flow.The initial yield of mannose is 27% or so, due to molybdenum
It is lost, after reaction 7 days, yield is down to 23% or so.After reaction 33, yield is down to 12% or so, and about 1/3 molybdenum is lost
(bibliography: Applied Catalysis A, 2008,334 (1-2): 112-118).
In addition, inventor also refers to the mode of embodiment 1-9, with the other raw materials and condition listed in this specification
Continuous flow reaction is successfully applied to etc. being tested, and also with the continuous flow catalytic reactor of the utility model.
Examples detailed above is only to illustrate the technical ideas and features of the present invention, and its object is to allow be familiar with technique
People is can to understand the content of the utility model and implement accordingly, is not limited the protection scope of the present invention.It is all
According to the spirit of the present invention substantially equivalent transformation that is done or modification, should all cover the protection scope of the utility model it
It is interior.
Claims (8)
1. a kind of continuous flow catalytic reactor, including reaction vessel and the filler being packaged in the reaction vessel；Its feature
Be: the continuous flow catalytic reactor further includes electrically charged catalyst component, and the catalyst component is under DC electric field effect
It is fixed on the filler.
2. continuous flow catalytic reactor according to claim 1, it is characterised in that: the reaction vessel is tubular structure.
3. continuous flow catalytic reactor according to claim 1, it is characterised in that: the reaction vessel is glass material
's.
4. continuous flow catalytic reactor according to claim 1, it is characterised in that: the filler includes active carbon, ion
The combination of any one or two kinds in exchanger resin.
5. continuous flow catalytic reactor according to claim 1, it is characterised in that: the catalyst component includes quantum dot,
The quantum dot includes molybdenum oxide quantum dot；Alternatively, the catalyst component includes molybdenum acid ion or ferric hydroxide colloid grain
Son.
6. continuous flow catalytic reactor according to claim 2, it is characterised in that: the internal diameter of the reaction vessel is 1.5
~2 centimetres, length is 50~80 centimetres, and volume is 100-200 milliliters.
7. continuous flow catalytic reactor according to claim 4, it is characterised in that: the particle size of the filler be 10~
50 mesh, and the mass volume ratio of the volume of the gross mass of the filler and the reaction vessel is 50~120 grams: 100~200
Milliliter.
8. continuous flow catalytic reactor according to claim 1, it is characterised in that: be used to form the straight of the DC electric field
The voltage in galvanic electricity source is 5~50 volts.
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| CN110961041A (en) * | 2018-09-29 | 2020-04-07 | 中国科学院宁波材料技术与工程研究所 | Continuous flow catalytic reactor, method of assembling same and use thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110961041A (en) * | 2018-09-29 | 2020-04-07 | 中国科学院宁波材料技术与工程研究所 | Continuous flow catalytic reactor, method of assembling same and use thereof |
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