CN117225331A - Microchannel reaction device for producing tartaric acid and preparation method - Google Patents
Microchannel reaction device for producing tartaric acid and preparation method Download PDFInfo
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- CN117225331A CN117225331A CN202311448223.XA CN202311448223A CN117225331A CN 117225331 A CN117225331 A CN 117225331A CN 202311448223 A CN202311448223 A CN 202311448223A CN 117225331 A CN117225331 A CN 117225331A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 632
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000011975 tartaric acid Substances 0.000 title claims abstract description 46
- 235000002906 tartaric acid Nutrition 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 137
- 239000003054 catalyst Substances 0.000 claims abstract description 111
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 38
- 239000011159 matrix material Substances 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 96
- 238000011049 filling Methods 0.000 claims description 52
- DCEMCPAKSGRHCN-UHFFFAOYSA-N oxirane-2,3-dicarboxylic acid Chemical compound OC(=O)C1OC1C(O)=O DCEMCPAKSGRHCN-UHFFFAOYSA-N 0.000 claims description 48
- 238000007599 discharging Methods 0.000 claims description 35
- 239000003377 acid catalyst Substances 0.000 claims description 32
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims description 32
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 27
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- 238000006460 hydrolysis reaction Methods 0.000 claims description 19
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 claims description 18
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000013461 design Methods 0.000 description 3
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- FEWJPZIEWOKRBE-LWMBPPNESA-N levotartaric acid Chemical compound OC(=O)[C@@H](O)[C@H](O)C(O)=O FEWJPZIEWOKRBE-LWMBPPNESA-N 0.000 description 3
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- FEWJPZIEWOKRBE-XIXRPRMCSA-N Mesotartaric acid Chemical compound OC(=O)[C@@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-XIXRPRMCSA-N 0.000 description 2
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Abstract
The invention provides a micro-channel reaction device for producing tartaric acid and a preparation method thereof, wherein the micro-channel reaction device comprises a top layer, a reaction layer and a bottom layer which are laminated in sequence and can be detachably fixed; the inside of the top layer is provided with a first heat exchange channel which is relatively closed, and the inside of the bottom layer is provided with a second heat exchange channel which is relatively closed; the reaction layer comprises a plurality of mutually independent micro-reaction modules which are arranged in a matrix, wherein each micro-reaction module is of a Z-shaped convex structure, a continuous folded line-shaped groove structure is formed between every two adjacent micro-reaction modules, and the groove structures are mutually communicated to form a reaction channel; at least two open holes are arranged on the side of the micro-reaction module, and the convex structures are communicated with the adjacent groove structures through the open holes so as to form a continuous flow passage of the reaction liquid; the interior of the groove structure is filled with a catalyst. The invention adopts the microchannel reaction device to prepare tartaric acid, improves the mass transfer driving force and the heat transfer driving force between the reaction raw materials, and greatly strengthens the mass transfer and heat transfer efficiency in the reaction process.
Description
Technical Field
The invention belongs to the technical field of tartaric acid production, and relates to a microchannel reaction device for producing tartaric acid and a preparation method thereof.
Background
Tartaric acid is an important chemical product, and is widely applied to industries such as food, medicine, light chemical industry, textile industry and the like, and also has important application in the fields such as telecommunication equipment, leather making, electroplating, printing and dyeing, glass ceramic and the like.
Tartaric Acid (TA), 2, 3-dihydroxysuccinic acid, with molecular formula C 4 H 6 O 6 Is an organic carboxylic acid which exists mainly in free state or acid salt form, is easy to dissolve in water and ethanol and is slightly soluble in diethyl ether. There are two exactly equivalent chiral carbon atoms in the tartaric acid molecule, so it has three optical isomers, namely, levotartaric acid (LTA), dextrorotataric acid (D-TA) and meso-tartaric acid (meso-TA). Of these, LTA and DTA are a pair of enantiomers, and an equal mixture of both is called racemic tartaric acid (DL-TA).
The DL-TA has very wide application, for example, can be used as an acidulant, has acidity 1.2-1.3 times higher than that of citric acid, has higher solubility and strong chelating ability for metal ions, can be used for various foods, and can be used in proper amount according to production needs. Can also be used in antioxidant synergists, tanning agents, chelating agents, complexing agents and medicaments, and can be widely used in the industrial fields of medicines, foods, leather making, chemical industry, textile industry and the like.
At present, four common industrial production methods of tartaric acid comprise an extraction method, a chemical synthesis method, a semisynthesis method and a fermentation method, but the four common synthesis methods have a plurality of defects, such as long reaction period, low product yield, difficult separation of a catalyst in a homogeneous system and the like, so that the method has great significance in researching and optimizing the synthesis process of DL-TA.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide the micro-channel reaction device for producing tartaric acid and the preparation method thereof.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a microchannel reaction apparatus for producing tartaric acid, the microchannel reaction apparatus comprising a top layer, a reaction layer and a bottom layer laminated in sequence and detachably fixed;
The inside of the top layer is provided with a first heat exchange channel which is relatively closed, and the inside of the bottom layer is provided with a second heat exchange channel which is relatively closed; a first heat exchange medium inlet and a first heat exchange medium outlet which are communicated with the first heat exchange channel are formed in the side edge of the top layer; a second heat exchange medium inlet and a second heat exchange medium outlet which are connected with the second heat exchange channel are formed in the side edge of the bottom layer;
three feeding channels and one discharging channel are formed in the top surface of the top layer, and the feeding channels and the discharging channels avoid the first heat exchange channel and are communicated with the reaction layer;
the reaction layer comprises a plurality of mutually independent micro-reaction modules which are arranged in a matrix, wherein each micro-reaction module is of a Z-shaped convex structure, a continuous folded line-shaped groove structure is formed between every two adjacent micro-reaction modules, and the groove structures are mutually communicated to form a reaction channel;
the side of the micro-reaction module is provided with at least two open holes, the convex structures are communicated with the adjacent groove structures through the open holes so as to form a continuous flow path of reaction liquid, and the reaction liquid flows into the groove structures from the convex structures or flows into the convex structures from the groove structures through the open holes;
The inside of the groove structure is filled with a catalyst.
The invention adopts the micro-channel reaction device to prepare tartaric acid, and the widths and depths of the micro-reaction modules and the reaction channels in the micro-channel reaction device are smaller, generally tens to hundreds of micrometers, and the micro-channel reaction device has shorter molecular diffusion distance and larger specific surface area, so that the physical quantity gradient, such as temperature gradient, concentration gradient, pressure gradient and the like, in the micro-channel reaction device can be rapidly increased, and the mass transfer driving force and the heat transfer driving force between reaction raw materials are improved by the physical quantity gradient; meanwhile, the larger specific surface area provides a larger reaction space for the mass transfer and heat transfer process of the reaction raw materials, so that the internal temperature distribution of the reaction layer can be uniform in a very short time, and the mass transfer and heat transfer efficiency in the reaction process is greatly enhanced. Compared with the conventional reaction device, the method for synthesizing the tartaric acid in the microchannel reaction device has the advantages of high reaction speed, less consumption of reaction raw materials, easy control of reaction process and the like.
According to the invention, through the optimal design of the configuration of the micro-reaction modules, the reaction raw materials can be quickly mixed and generate transverse flow when passing through each micro-reaction module, so that the chaotic mixing effect of the cooperation of the droplet flow and the layering flow is further induced, a turbulent vortex is formed in the reaction channel, and the mixing effect and the mass transfer efficiency of the reaction raw materials are greatly improved.
In the invention, the reaction raw materials have two different flow states of stratified flow and liquid drop flow at the same time, which are caused by different flow rates of different areas in the reaction channel and the micro-reaction module. The invention adopts the zigzag micro-reaction module, so that when the reaction raw materials flow into the micro-reaction module, the flow speed of the reaction raw materials in the protruding structure of the micro-reaction module is slowed down due to the zigzag baffling effect; the reaction raw materials can still keep high flow velocity in the reaction channels of the groove structures between the adjacent micro-reaction modules. The reaction channels of the micro-reaction modules of the convex structures and the groove structures promote the reaction raw materials to form different flowing states, layering flows are generated in the micro-reaction modules of the convex structures, and drop streams are generated in the reaction channels of the groove structures. On the basis, the micro-reaction module with the convex structure is communicated with the reaction channel with the concave structure through the opening on the side edge of the micro-reaction module, so that the reaction raw material repeatedly flows between the micro-reaction module and the reaction channel, and the flowing state of the reaction raw material is repeatedly switched between the flowing state of the liquid drop flow and the flowing state of the layering flow in the process of repeatedly flowing, thereby improving the mixing degree of the reaction raw materials and enhancing the liquid-liquid mass transfer efficiency among different reaction raw materials.
After the conventional catalytic reaction is finished, the reaction product is usually required to be separated from the catalyst, but direct separation of the reaction product and the catalyst is difficult to realize in a microchannel feedback device; in addition, in order to ensure smooth progress of the catalytic reaction, it is necessary to sufficiently contact the reaction raw materials with the catalyst. Therefore, the catalyst is directly filled into the groove structure in the form of the filler, so that the catalyst filler layer with high specific surface area is obtained, the catalyst filler layer can be directly and fully contacted with the catalyst when the reaction raw material flows through the reaction channel of the groove structure, and the contact area of the reaction raw material and the catalyst can be increased, so that the reaction rate is accelerated; and the technical problem that the reaction raw materials and the catalyst are difficult to separate can be effectively solved. In addition, the catalyst filler can also be used as a shearing filler in the reaction channel to shear and disperse the reaction raw materials flowing through the catalyst filler, so that the droplet diameter of the reaction raw materials is further reduced, the mixing effect and the effective contact area between the reaction raw materials are improved, and the liquid-liquid mass transfer efficiency between the reaction raw materials is greatly improved.
As a preferable technical scheme of the invention, the micro-channel reaction device is of a rectangular structure with long sides and wide sides, the wide sides of the micro-channel reaction device are defined as x-direction, the long sides of the micro-channel reaction device are defined as y-direction, and a plurality of micro-reaction modules are respectively distributed at equal intervals along the x-direction and the y-direction.
The two ends of the reaction layer in the y direction are also respectively provided with a liquid inlet tank and a liquid outlet tank, and the liquid inlet tank and the liquid outlet tank are respectively communicated with the two ends of the reaction channel in the y direction.
The three feed channels are a first feed channel, a second feed channel and a third feed channel which are arranged along the x direction respectively, the feed ends of the first feed channel, the second feed channel and the third feed channel are positioned on the surface of the top layer, the outlet ends of the first feed channel, the second feed channel and the third feed channel are positioned in the reaction layer and are communicated with the liquid inlet tank, deionized water, maleic anhydride and hydrogen peroxide enter the liquid inlet tank through the first feed channel, the second feed channel and the third feed channel respectively, and flow into the reaction channel after being mixed in the liquid inlet tank.
And the inlet end of the discharging channel is communicated with the liquid outlet tank, and reaction products obtained by the reaction in the reaction channel are collected into the liquid outlet tank and discharged through the discharging channel.
The outlet end of the discharging channel is connected with a liquid collecting bottle; the liquid collecting bottle is externally connected with a vacuumizing device, and the vacuumizing device is used for vacuumizing the liquid collecting bottle so as to suck reaction products in the liquid outlet pool into the liquid collecting bottle through the discharging channel; the liquid collecting bottle is further provided with a pressure regulating valve and a vacuum gauge, the pressure regulating valve is used for regulating negative pressure in the liquid collecting bottle, and the vacuum gauge is used for monitoring vacuum degree in the liquid collecting bottle.
The invention adopts negative pressure sample injection, vacuumizes the liquid collecting bottle through the vacuumizing device, sucks the reaction raw materials into the reaction layer under the action of negative pressure, and reacts in the micro-reaction module and the reaction channel. The opening degree of the pressure regulating valve is regulated to control the vacuum degree in the liquid collecting bottle, so that the flow rate of the reaction raw materials flowing through the reaction layer is regulated. Since the volume of the liquid collection bottle is much larger than the dead volume of the microchannel reactor and the volume of the reaction raw material flowing through the reaction layer during the reaction, the reaction raw material can flow through the reaction layer at a stable flow rate. In addition, the negative pressure sampling mode adopted by the invention only adopts one vacuumizing device, so that various reaction raw materials can be simultaneously driven to enter the reaction layer from different feeding channels, and the cost of driving equipment is greatly reduced.
As a preferable technical scheme of the invention, the micro-reaction module is divided into a first transverse bulge, a longitudinal bulge and a second transverse bulge which are communicated in sequence, wherein the first transverse bulge and the second transverse bulge are parallel to the x direction, and the longitudinal bulge is parallel to the y direction.
The two ends of the first transverse bulge in the x direction are a first transverse end and a second transverse end respectively, the two ends of the longitudinal bulge in the y direction are a first longitudinal end and a second longitudinal end respectively, and the two ends of the second transverse bulge in the x direction are a third transverse end and a fourth transverse end respectively.
The first transverse end is provided with a first opening, the second transverse end is vertically abutted with the first longitudinal end, the second longitudinal end is vertically abutted with the third transverse end, and the fourth transverse end is provided with a second opening.
The reaction raw materials enter the micro-reaction module through the first opening, and flow out from the second opening along the first transverse bulge, the longitudinal bulge and the second transverse bulge in sequence; or the micro-reaction module enters from the second opening, and flows out from the first opening along the second transverse bulge, the longitudinal bulge and the first transverse bulge in sequence.
As a preferable technical scheme of the invention, the first heat exchange channel and the second heat exchange channel are both in a serpentine structure, and after the heat exchange medium enters the first heat exchange channel, the heat exchange medium flows from one end to the other end along the x direction and returns back to the other end, and is pushed in a serpentine manner along the y direction; after the heat exchange medium enters the second heat exchange channel, one end of the heat exchange medium flows to the other end along the y direction, and the heat exchange medium returns back to the other end and is pushed in a serpentine manner along the x direction.
The first heat exchange medium inlet and the first heat exchange medium outlet are positioned on the same side edge of the top layer in the y direction or respectively positioned on two opposite side edges of the top layer in the y direction; the second heat exchange medium inlet and the second heat exchange medium outlet are positioned on the same side of the top layer in the x direction or respectively positioned on two opposite sides of the top layer in the x direction.
As a preferable technical scheme of the invention, the first heat exchange channel and the second heat exchange channel are both in a serpentine structure, and after the heat exchange medium enters the first heat exchange channel, the heat exchange medium flows from one end to the other end along the y direction and returns back to the other end, and is pushed in a serpentine manner along the x direction; after the heat exchange medium enters the second heat exchange channel, one end of the heat exchange medium flows to the other end along the x direction, and the heat exchange medium returns back to the other end and is pushed in a serpentine manner along the y direction.
The first heat exchange medium inlet and the first heat exchange medium outlet are positioned on the same side of the top layer in the x direction or respectively positioned on two opposite sides of the top layer in the x direction; the second heat exchange medium inlet and the second heat exchange medium outlet are positioned on the same side of the top layer in the y direction or respectively positioned on two opposite sides of the top layer in the y direction.
As a preferable technical scheme of the invention, the reaction channel is divided into a first reaction section, a second reaction section and a third reaction section with unequal lengths along the y direction, wherein the length of the third reaction section in the y direction is less than that of the first reaction section in the y direction and less than that of the second reaction section in the y direction.
The length of the first reaction section in the y direction is 15-30% of the total length of the reaction channel, for example, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29% or 30%; the length of the second reaction section in the y direction is 60-80% of the total length of the reaction channel, for example, 60%, 62%, 64%, 66%, 68%, 70%, 72%, 74%, 76%, 78% or 80%; the length of the third reaction section in the y direction is 5 to 10% of the total length of the reaction channel, for example, 5.0%, 5.5%, 6.0%, 6.5%, 7.0%, 7.5%, 8.0%, 8.5%, 9.0%, 9.5% or 10.0%, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
As a preferred embodiment of the present invention, the distance between the longitudinal projections of two adjacent microreaction modules in the x-direction is the channel pitch.
The channel spacing in the first reaction section is the same, the channel spacing in the second reaction section is the same, the channel spacing in the first reaction section is less than the channel spacing in the third reaction section is less than the channel spacing in the second reaction section.
The ratio of the channel spacing of the first, second and third reaction sections is 1 (1.5-2): (1.3-1.6), which may be, for example, but not limited to, 1:1.5:1.3, 1:1.55:1.35, 1:1.6:1.4, 1:1.65:1.45, 1:1.7:1.5, 1:1.75:1.55, 1:1.8:1.6, 1:1.85:1.3, 1:1.9:1.4, 1:1.95:1.5 or 1:1.6:2, other non-enumerated values within this range of values are equally applicable.
The channel spacing in the reaction layer has obvious influence on the liquid-liquid mass transfer coefficient and the average diameter of liquid drops of the reaction raw materials, and the micro-reaction module can generate stronger shearing force along with the reduction of the channel spacing, so that the liquid-liquid mass transfer coefficient is increased; further, as the channel pitch decreases, the average diameter of the droplets of the reaction raw material decreases, so that the contact area between the reaction raw materials increases.
The invention optimizes the channel spacing of each region in the reaction layer aiming at the tartaric acid production process, thereby realizing the regulation and control of the flow rate, the dispersion degree, the flowing state and the particle size of the reaction raw materials and further meeting the requirements of the tartaric acid production process on the state of the reaction raw materials at different stages.
In the invention, the channel spacing in the first reaction section is minimum, the reaction raw material takes the liquid drop flow as the main material, the average diameter of the liquid drop of the reaction raw material is smaller, the liquid drop generation speed is higher, the liquid drop size of the reaction raw material is approximately in a disperse phase in the micro-reaction module and the reaction channel of the first reaction section, the liquid drop size of the reaction raw material is larger than the characteristic size of the reaction channel, a plurality of relatively independent reaction raw material liquid columns are formed in the reaction channel and the micro-reaction module under the shearing action of the wall of the reaction channel on the liquid drop, chaotic flow formed by transverse flow and longitudinal flow is generated between the reaction raw material liquid columns, meanwhile, the inner circulation flow is generated in the reaction raw material liquid column, the joint action of the chaotic flow and the inner circulation flow reduces the boundary layer thickness and the molecular diffusion distance of the reaction raw material liquid column, the contact area and the interface updating speed of the reaction raw material liquid column are increased, and the mass transfer efficiency of the reaction raw material is enhanced, so that the rapid mixing and the rapid mass transfer between the reaction raw materials are realized in the first reaction section.
The channel spacing in the second reaction section is the largest, in the second reaction section, the reaction raw material is mainly stratified flow, the average diameter of liquid drops of the reaction raw material is larger, the generation speed of the liquid drops is slower, the reaction raw material is continuous in the micro-reaction module of the second reaction section and the reaction channel, meanwhile, the reaction liquid raw material does not have internal circulation flow in the second reaction section, the mass transfer mode between the reaction liquid raw materials is mainly molecular diffusion, the reaction liquid raw material can be in close contact with the catalyst filler in the second reaction section in molecular level, and the contact area between the reaction raw material and the catalyst is improved; in addition, the flow rate of the reaction raw materials in the second reaction section is slowest, so that the contact time of the reaction raw materials and the catalyst filler can be prolonged to the greatest extent, the catalytic reaction is ensured to be completely carried out, the reaction rate is greatly improved, and all the reaction raw materials can be fully reacted.
The space between channels in the third reaction section is between the first reaction section and the second reaction section, the third reaction section has the function of carrying out high-temperature hydrolysis on the reaction liquid obtained by the reaction in the second reaction section, and the temperature required by the hydrolysis reaction needs to be higher than the temperature required by the catalytic reaction in the second reaction section, the temperature of the catalytic reaction in the second reaction section is controlled to be 70-80 ℃, the hydrolysis reaction in the third reaction section needs to be 100-110 ℃, but the temperatures of heat exchange media flowing in the top layer and the bottom layer are consistent everywhere, and the temperature of the third reaction section cannot be independently controlled by independently regulating the temperature of the heat exchange media at different positions of the heat exchange channels, so that the heat transfer efficiency and the heat preservation effect of the third reaction section can be improved only on the premise that the temperature of the heat exchange media is kept unchanged, and the reaction liquid in the third reaction section can obtain more heat to reach the temperature condition of the hydrolysis reaction. Therefore, the invention adjusts the channel spacing of the third reaction section so as to control the flowing state of the reaction liquid in the third reaction section, so that two flowing states of stratified flow and liquid drop flow alternately appear when the reaction liquid passes between the micro-reaction module and the reaction channel, the duty ratio of the two flowing states is kept balanced, and relative movement is generated between different flowing lines on a flowing interface under the combined action of the two flowing states, thereby improving the contact area between the reaction liquid, reducing the thickness of a temperature boundary layer of the reaction liquid, shortening the heat exchange path of heat exchange media of a top layer and a bottom layer, enabling the reaction liquid in the third reaction section to receive more heat of the heat exchange media, and compared with the first reaction section and the second reaction section, the reaction temperature in the third reaction section is greatly improved; in addition, a small amount of catalyst filler is further arranged in the third reaction section, so that the catalytic effect can be continuously exerted on one hand, more importantly, a small amount of catalyst filler dispersed in the third reaction section can play a role of a static mixing piece, when the reaction liquid flows through the catalyst filler, the catalyst filler can produce a cutting effect on the reaction liquid, so that the reaction liquid rearranges and is combined again, the effect increases the contact area between the reaction liquids, and meanwhile, the effect of stretching, deforming and folding the reaction liquid microelements is accompanied, so that the update iteration between the inside and the surface layer of the reaction liquid is accelerated, and the temperature of each part of the reaction liquid is uniform and stable in a short time, so that the progress of hydrolysis reaction is accelerated.
As a preferable technical scheme of the invention, the catalyst filling amount in the first reaction section is equal everywhere, the catalyst filling amount in the second reaction section is equal everywhere, the catalyst filling amount in the third reaction section is equal everywhere, and the catalyst filling amount of the first reaction section < the catalyst filling amount of the third reaction section < the catalyst filling amount of the second reaction section.
The first reaction section is not filled with catalyst, and the catalyst filling amount in the second reaction section is 70-80wt% of the total catalyst filling amount, for example, 70wt%, 71wt%, 72wt%, 73wt%, 74wt%, 75wt%, 76wt%, 77wt%, 78wt%, 79wt% or 80wt%; the catalyst loading in the third reaction zone is 20-30wt% of the total catalyst loading, and may be, for example, 20wt%, 21wt%, 22wt%, 23wt%, 24wt%, 25wt%, 26wt%, 27wt%, 28wt%, 29wt% or 30wt%, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In a second aspect, the present invention provides a method for preparing tartaric acid, the method being carried out in the microchannel reaction device according to the first aspect, the method comprising:
Filling a tungstic acid catalyst in the groove structure, and introducing heat exchange media into the first heat exchange channel and the second heat exchange channel to heat the reaction layer;
(II) respectively injecting deionized water, maleic anhydride and hydrogen peroxide solution into the micro-channel reaction device through different feed channels, mixing reaction raw materials in the reaction channels and the micro-reaction module, and reacting under the action of a tungstic acid catalyst to generate epoxy succinic acid solution when flowing through a tungstic acid catalyst filling layer;
and (III) discharging the epoxy succinic acid solution from the micro-channel reaction device through a discharging channel, cooling and self-crystallizing the epoxy succinic acid solution, and then performing suction filtration to obtain crystals, wherein the crystals are dried to obtain the tartaric acid.
In a preferred embodiment of the present invention, in the step (I), the temperature of the heat exchange medium is 100 to 120. DegreeC, for example, 100. DegreeC, 102. DegreeC, 104. DegreeC, 106. DegreeC, 108. DegreeC, 110. DegreeC, 112. DegreeC, 114. DegreeC, 116. DegreeC, 118. DegreeC or 120. DegreeC, but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value range are applicable.
The mass ratio of the tungstic acid catalyst to the maleic anhydride is (0.005-0.01): 1, for example, may be 0.005:1, 0.0055:1, 0.006:1, 0.0065:1, 0.007:1, 0.0075:1, 0.008:1, 0.0085:1, 0.009:1, 0.0095:1 or 0.01:1, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In the step (II), the mass ratio of deionized water, maleic anhydride and hydrogen peroxide is 1 (0.9-1): (1.4-1.6), for example, may be 1:0.9:1.4, 1:0.91:1.42, 1:0.92:1.44, 1:0.93:1.46, 1:0.94:1.48, 1:0.95:1.5, 1:0.96:1.52, 1:0.97:1.54, 1:0.98:1.56, 1:0.99:1.58 or 1:1:1.6, but not limited to the recited values, and other non-recited values in the numerical range are equally applicable.
The mass fraction of the hydrogen peroxide solution is 25-30wt%, and may be, for example, 25wt%, 25.5wt%, 26wt%, 26.5wt%, 27wt%, 27.5wt%, 28wt%, 28.5wt%, 29wt%, 29.5wt%, or 30wt%, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In the step (III), the reaction temperature of the heated hydrolysis is 105 to 115℃and may be, for example, 105℃106℃107℃108℃109℃110℃111℃112℃113℃114℃115℃but not limited to the values listed, and other values not listed in the range are equally applicable.
The reaction time of the thermal hydrolysis is 3 to 4 hours, and may be, for example, 3.0 hours, 3.1 hours, 3.2 hours, 3.3 hours, 3.4 hours, 3.5 hours, 3.6 hours, 3.7 hours, 3.8 hours, 3.9 hours or 4.0 hours, but is not limited to the recited values, and other non-recited values within the range are equally applicable. The temperature of the cooling is 5 to 10 ℃, for example, 5.0 ℃, 5.5 ℃, 6.0 ℃, 6.5 ℃, 7.0 ℃, 7.5 ℃, 8.0 ℃, 8.5 ℃, 9.0 ℃, 9.5 ℃ or 10.0 ℃, but the temperature is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts the micro-channel reaction device to prepare tartaric acid, and the widths and depths of the micro-reaction modules and the reaction channels in the micro-channel reaction device are smaller, generally tens to hundreds of micrometers, and the micro-channel reaction device has shorter molecular diffusion distance and larger specific surface area, so that the physical quantity gradient, such as temperature gradient, concentration gradient, pressure gradient and the like, in the micro-channel reaction device can be rapidly increased, and the mass transfer driving force and the heat transfer driving force between reaction raw materials are improved by the physical quantity gradient; meanwhile, the larger specific surface area provides a larger reaction space for the mass transfer and heat transfer process of the reaction raw materials, so that the internal temperature distribution of the reaction layer can be uniform in a very short time, and the mass transfer and heat transfer efficiency in the reaction process is greatly enhanced. Compared with the conventional reaction device, the method for synthesizing the tartaric acid in the microchannel reaction device has the advantages of high reaction speed, less consumption of reaction raw materials, easy control of reaction process and the like.
According to the invention, through the optimal design of the configuration of the micro-reaction modules, the reaction raw materials can be quickly mixed and generate transverse flow when passing through each micro-reaction module, so that the chaotic mixing effect of the cooperation of the droplet flow and the layering flow is further induced, a turbulent vortex is formed in the reaction channel, and the mixing effect and the mass transfer efficiency of the reaction raw materials are greatly improved.
In the invention, the reaction raw materials have two different flow states of stratified flow and liquid drop flow at the same time, which are caused by different flow rates of different areas in the reaction channel and the micro-reaction module. The invention adopts the zigzag micro-reaction module, so that when the reaction raw materials flow into the micro-reaction module, the flow speed of the reaction raw materials in the protruding structure of the micro-reaction module is slowed down due to the zigzag baffling effect; the reaction raw materials can still keep high flow velocity in the reaction channels of the groove structures between the adjacent micro-reaction modules. The reaction channels of the micro-reaction modules of the convex structures and the groove structures promote the reaction raw materials to form different flowing states, layering flows are generated in the micro-reaction modules of the convex structures, and drop streams are generated in the reaction channels of the groove structures. On the basis, the micro-reaction module with the convex structure is communicated with the reaction channel with the concave structure through the opening on the side edge of the micro-reaction module, so that the reaction raw material repeatedly flows between the micro-reaction module and the reaction channel, and the flowing state of the reaction raw material is repeatedly switched between the flowing state of the liquid drop flow and the flowing state of the layering flow in the process of repeatedly flowing, thereby improving the mixing degree of the reaction raw materials and enhancing the liquid-liquid mass transfer efficiency among different reaction raw materials.
After the conventional catalytic reaction is finished, the reaction product is usually required to be separated from the catalyst, but direct separation of the reaction product and the catalyst is difficult to realize in a microchannel feedback device; in addition, in order to ensure smooth progress of the catalytic reaction, it is necessary to sufficiently contact the reaction raw materials with the catalyst. Therefore, the catalyst is directly filled into the groove structure in the form of the filler, so that the catalyst filler layer with high specific surface area is obtained, the catalyst filler layer can be directly and fully contacted with the catalyst when the reaction raw material flows through the reaction channel of the groove structure, and the contact area of the reaction raw material and the catalyst can be increased, so that the reaction rate is accelerated; and the technical problem that the reaction raw materials and the catalyst are difficult to separate can be effectively solved. In addition, the catalyst filler can also be used as a shearing filler in the reaction channel to shear and disperse the reaction raw materials flowing through the catalyst filler, so that the droplet diameter of the reaction raw materials is further reduced, the mixing effect and the effective contact area between the reaction raw materials are improved, and the liquid-liquid mass transfer efficiency between the reaction raw materials is greatly improved.
Drawings
FIG. 1 is a schematic structural view of a microchannel reactor according to an embodiment of the present invention;
FIG. 2 is a schematic view showing the appearance of a microchannel reactor according to an embodiment of the present application;
FIG. 3 is a schematic view showing the internal structure of a reaction layer of a microchannel reactor according to an embodiment of the application;
FIG. 4 is a top view of a reaction layer of a microchannel reactor according to one embodiment of the application;
wherein, 1-top layer; 2-a reaction layer; 3-bottom layer; 4-a first feed channel; 5-a second feed channel; 6-a third feed channel; 7-a discharge channel; 8-a first heat exchange channel; 9-a first heat exchange medium inlet; 10-a first heat exchange medium outlet; 11-a second heat exchange channel; 12-a second heat exchange medium inlet; 13-a second heat exchange medium outlet; 14-feeding a liquid pool; 15-discharging the liquid pool; 16-reaction channel; 17-a microreaction module; 18-a first reaction zone; 19-a second reaction section; 20-a third reaction section; 21-a catalyst filler; 22-a first lateral projection; 23-longitudinal protrusions; 24-a second lateral protrusion; 25-a first opening; 26-a second opening; 27-vacuumizing device; 28-collecting liquid bottle; 29-a pressure regulating valve; 30-vacuum gauge.
Detailed Description
The technical scheme of the application is described in detail below with reference to specific embodiments and attached drawings. The examples described herein are specific embodiments of the present application for illustrating the concept of the present application; the description is intended to be illustrative and exemplary in nature and should not be construed as limiting the scope of the application in its aspects. In addition to the embodiments described herein, those skilled in the art can adopt other obvious solutions based on the disclosure of the claims and the specification thereof, including those adopting any obvious substitutions and modifications to the embodiments described herein.
In one embodiment, the invention provides a microchannel reaction device for producing tartaric acid, which comprises a top layer 1, a reaction layer 2 and a bottom layer 3 which are sequentially laminated and detachably fixed as shown in fig. 1;
the inside of the top layer 1 is provided with a first heat exchange channel 8 which is relatively closed, and the inside of the bottom layer 3 is provided with a second heat exchange channel 11 which is relatively closed;
the side edge of the top layer 1 is provided with a first heat exchange medium inlet 9 and a first heat exchange medium outlet 10 which are communicated with the first heat exchange channel 8; the side edge of the bottom layer 3 is provided with a second heat exchange medium inlet 12 and a second heat exchange medium outlet 13 which are connected with the second heat exchange channel 11;
three feeding channels and one discharging channel 7 are formed in the top surface of the top layer 1, and the feeding channels and the discharging channel 7 avoid the first heat exchange channel 8 and are communicated with the reaction layer 2;
the reaction layer 2 comprises a plurality of mutually independent micro-reaction modules 17 which are arranged in a matrix, the micro-reaction modules 17 are of Z-shaped convex structures, continuous folded linear groove structures are formed between adjacent micro-reaction modules 17, and the groove structures are mutually communicated to form a reaction channel 16;
at least two openings are arranged on the side of the micro-reaction module 17, the convex structures are communicated with the adjacent groove structures through the openings so as to form a continuous flow path of the reaction liquid, and the reaction liquid flows into the groove structures through the openings or flows into the convex structures through the groove structures; the interior of the groove structure is filled with a catalyst.
The invention adopts the micro-channel reaction device to prepare tartaric acid, and the widths and depths of the micro-reaction module 17 and the reaction channel 16 in the micro-channel reaction device are smaller, generally tens to hundreds of micrometers, and the micro-channel reaction device has shorter molecular diffusion distance and larger specific surface area, so that the physical quantity gradient, such as temperature gradient, concentration gradient, pressure gradient and the like, in the micro-channel reaction device can be rapidly increased, and the mass transfer driving force and the heat transfer driving force between reaction raw materials are improved by the physical quantity gradient; meanwhile, the larger specific surface area provides a larger reaction space for the mass and heat transfer process of the reaction raw materials, so that the internal temperature distribution of the reaction layer 2 can be uniform in a very short time, and the mass and heat transfer efficiency in the reaction process is greatly enhanced. Compared with the conventional reaction device, the method for synthesizing the tartaric acid in the microchannel reaction device has the advantages of high reaction speed, less consumption of reaction raw materials, easy control of reaction process and the like.
According to the invention, through the optimal design of the configuration of the micro-reaction modules 17, the reaction raw materials can be quickly mixed and generate transverse flow when passing through each micro-reaction module 17, so that the chaotic mixing effect of the synergy of the droplet flow and the layering flow is further induced, a turbulent vortex is formed in the reaction channel 16, and the mixing effect and the mass transfer efficiency of the reaction raw materials are greatly improved.
In the present invention, the two different flow states of the stratified flow and the droplet flow exist at the same time, which are caused by the different flow rates of different regions in the reaction channel 16 and the micro-reaction module 17. The invention adopts the Z-shaped micro-reaction module 17, so that when the reaction raw materials flow into the micro-reaction module 17, the flow speed of the reaction raw materials in the convex structure of the micro-reaction module 17 is slowed down due to the Z-shaped baffling effect; the reaction raw materials can still maintain a high flow rate in the reaction channels 16 of the groove structures between the adjacent micro-reaction modules 17. The reaction channels 16 of the raised micro-reaction modules 17 and the recessed micro-reaction modules 17 promote different flow conditions of the reaction materials, and a stratified flow is generated in the raised micro-reaction modules 17, while a droplet flow is generated in the recessed micro-reaction channels 16. On the basis, the micro-reaction module 17 with the convex structure is communicated with the reaction channel 16 with the concave structure through the opening on the side edge of the micro-reaction module 17, so that the reaction raw materials repeatedly flow between the micro-reaction module 17 and the reaction channel 16, and the flowing state of the reaction raw materials is repeatedly switched between the flowing state of the liquid drop flow and the flowing state of the stratified flow in the process of repeatedly flowing, thereby improving the mixing degree of the reaction raw materials and enhancing the liquid-liquid mass transfer efficiency among different reaction raw materials.
After the conventional catalytic reaction is finished, the reaction product is usually required to be separated from the catalyst, but direct separation of the reaction product and the catalyst is difficult to realize in a microchannel feedback device; in addition, in order to ensure smooth progress of the catalytic reaction, it is necessary to sufficiently contact the reaction raw materials with the catalyst. Therefore, the catalyst is directly filled into the groove structure in the form of the filler, so that the catalyst filler layer with high specific surface area is obtained, the catalyst filler layer can be directly and fully contacted with the catalyst when the reaction raw material flows through the reaction channel of the groove structure, and the contact area of the reaction raw material and the catalyst can be increased, so that the reaction rate is accelerated; and the technical problem that the reaction raw materials and the catalyst are difficult to separate can be effectively solved. In addition, the catalyst filler 21 can also be used as a shearing filler in the reaction channel 16 to shear and disperse the reaction raw materials flowing through the catalyst filler, so that the droplet diameter of the reaction raw materials is further reduced, the mixing effect and the effective contact area between the reaction raw materials are improved, and the liquid-liquid mass transfer efficiency between the reaction raw materials is greatly improved.
In some alternative embodiments, the microchannel reactor is a rectangular structure having long sides and wide sides, the wide sides of the microchannel reactor being defined as the x-direction, the long sides of the microchannel reactor being defined as the y-direction, and the plurality of microreaction modules 17 being equally spaced along the x-direction and the y-direction, respectively.
In the embodiment shown in fig. 3, the two ends of the reaction layer 2 in the y direction are further provided with a liquid inlet tank 14 and a liquid outlet tank 15, respectively, and the liquid inlet tank 14 and the liquid outlet tank 15 are respectively communicated with the two ends of the reaction channel 16 in the y direction.
In the embodiment shown in fig. 2, the three feeding channels are a first feeding channel 4, a second feeding channel 5 and a third feeding channel 6 which are respectively arranged along the x direction, the feeding ends of the first feeding channel 4, the second feeding channel 5 and the third feeding channel 6 are positioned on the surface of the top layer 1, the outlet ends of the first feeding channel 4, the second feeding channel 5 and the third feeding channel 6 are positioned in the reaction layer 2 and are communicated with a liquid inlet tank 14, deionized water, maleic anhydride and hydrogen peroxide enter the liquid inlet tank 14 through the first feeding channel 4, the second feeding channel 5 and the third feeding channel 6 respectively, and flow into the reaction channel 16 after being mixed in the liquid inlet tank 14.
The inlet end of the discharging channel 7 is communicated with the liquid outlet tank 15, and reaction products obtained by the reaction in the reaction channel 16 are collected in the liquid outlet tank 15 and discharged through the discharging channel 7.
The outlet end of the discharging channel 7 is connected with a liquid collecting bottle 28; the liquid collecting bottle 28 is externally connected with a vacuumizing device 27, and the vacuumizing device 27 is used for vacuumizing the liquid collecting bottle 28 so as to suck reaction products in the liquid outlet tank 15 into the liquid collecting bottle 28 through the discharging channel 7; the liquid collecting bottle 28 is also provided with a pressure regulating valve 29 and a vacuum gauge 30, the pressure regulating valve 29 is used for regulating the negative pressure in the liquid collecting bottle 28, and the vacuum gauge 30 is used for monitoring the vacuum degree in the liquid collecting bottle 28.
The invention adopts negative pressure sample injection, the liquid collection bottle 28 is vacuumized through the vacuumizing device 27, the reaction raw materials are sucked into the reaction layer 2 under the action of negative pressure, and the reaction occurs in the micro-reaction module 17 and the reaction channel 16. By adjusting the opening of the pressure regulating valve 29, the degree of vacuum in the liquid collecting bottle 28 can be controlled, and the flow rate of the reaction raw material flowing through the reaction layer 2 can be adjusted. Since the volume of the liquid collection bottle 28 is much larger than the dead volume of the microchannel reactor and the volume of the reaction raw material flowing through the reaction layer 2 during the reaction, the reaction raw material can flow through the reaction layer 2 at a stable flow rate. In addition, the negative pressure sample injection mode adopted by the invention only adopts one vacuumizing device 27, so that various reaction raw materials can be simultaneously driven to enter the reaction layer 2 from different feed channels, and the cost of driving equipment is greatly reduced.
As a preferred embodiment of the present invention, the micro-reaction module 17 is divided into a first lateral protrusion 22, a longitudinal protrusion 23 and a second lateral protrusion 24, which are sequentially connected, wherein the first lateral protrusion 22 and the second lateral protrusion 24 are parallel to the x-direction, and the longitudinal protrusion 23 is parallel to the y-direction.
In the embodiment shown in fig. 4, the first lateral protrusion 22 has a first lateral end and a second lateral end at both ends in the x direction, the longitudinal protrusion 23 has a first longitudinal end and a second longitudinal end at both ends in the y direction, and the second lateral protrusion 24 has a third lateral end and a fourth lateral end at both ends in the x direction.
The first transverse end is provided with a first opening 25, the second transverse end is vertically butted with the first longitudinal end, the second longitudinal end is vertically butted with the third transverse end, and the fourth transverse end is provided with a second opening 26.
The reaction raw materials enter the micro-reaction module 17 through the first holes 25, and flow out from the second holes 26 along the first transverse protrusions 22, the longitudinal protrusions 23 and the second transverse protrusions 24 in sequence; or from the second opening 26 into the microreaction module 17 and out of the first opening 25 along the second lateral projection 24, the longitudinal projection 23 and the first lateral projection 22 in this order.
In some alternative embodiments, the first heat exchange channel 8 and the second heat exchange channel 11 are both in a serpentine structure, and after the heat exchange medium enters the first heat exchange channel 8, the heat exchange medium flows from one end to the other end along the x direction, and returns back to the other end, and serpentine pushing is performed along the y direction; after entering the second heat exchange channel 11, the heat exchange medium flows from one end to the other end along the y direction, returns back at the other end, and is pushed in a serpentine manner along the x direction.
In the embodiment as in fig. 1, the first heat exchange medium inlet 9 and the first heat exchange medium outlet 10 are located on the same side of the top layer 1 in the y direction or on opposite sides of the top layer 1 in the y direction, respectively; the second heat exchange medium inlet 12 and the second heat exchange medium outlet 13 are located on the same side of the top layer 1 in the x direction or on opposite sides of the top layer 1 in the x direction, respectively.
In some alternative embodiments, the first heat exchange channel 8 and the second heat exchange channel 11 are both in a serpentine structure, and after the heat exchange medium enters the first heat exchange channel 8, the heat exchange medium flows from one end to the other end along the y direction, and returns back to the other end, and serpentine pushing is performed along the x direction; after entering the second heat exchange channel 11, the heat exchange medium flows from one end to the other end along the x direction, returns back at the other end, and is pushed in a serpentine manner along the y direction.
The first heat exchange medium inlet 9 and the first heat exchange medium outlet 10 are positioned on the same side of the top layer 1 in the x direction or respectively positioned on two opposite sides of the top layer 1 in the x direction; the second heat exchange medium inlet 12 and the second heat exchange medium outlet 13 are located on the same side of the y-direction of the top layer 1 or on opposite sides of the y-direction of the top layer 1, respectively.
In some alternative embodiments, the reaction channel 16 is divided into a first reaction section 18, a second reaction section 19 and a third reaction section 20 of unequal lengths along the y-direction, the length of the third reaction section 20 in the y-direction < the length of the first reaction section 18 in the y-direction < the length of the second reaction section 19 in the y-direction.
Specifically, the length of the first reaction section 18 in the y direction is 15-30% of the total length of the reaction channel 16, the length of the second reaction section 19 in the y direction is 60-80% of the total length of the reaction channel 16, and the length of the third reaction section 20 in the y direction is 5-10% of the total length of the reaction channel 16.
In some alternative embodiments, the distance between the longitudinal projections 23 of two microreaction modules 17 adjacent in the x-direction is the channel spacing. In the embodiment shown in fig. 4, the channel spacing in the first reaction section 18 is the same, the channel spacing in the second reaction section 19 is the same, the channel spacing in the first reaction section 18 < the channel spacing in the third reaction section 20 < the channel spacing in the second reaction section 19.
Specifically, the ratio of the channel pitches of the first reaction section 18, the second reaction section 19 and the third reaction section 20 is 1 (1.5-2): 1.3-1.6.
The channel spacing in the reaction layer 2 has a significant effect on the liquid-liquid mass transfer coefficient and the average diameter of the droplets of the reaction raw material, and as the channel spacing decreases, the micro-reaction module 17 can generate stronger shear force, so that the liquid-liquid mass transfer coefficient increases; further, as the channel pitch decreases, the average diameter of the droplets of the reaction raw material decreases, so that the contact area between the reaction raw materials increases.
The invention optimizes the channel spacing of each region in the reaction layer 2 aiming at the tartaric acid production process, thereby realizing the regulation and control of the flow rate, the dispersion degree, the flowing state and the particle size of the reaction raw materials and further meeting the requirements of the tartaric acid production process on the state of the reaction raw materials at different stages.
In the invention, as shown in fig. 4, the channel spacing in the first reaction section 18 is the smallest, in the first reaction section 18, the reaction raw material is mainly droplet flow, the average diameter of droplets of the reaction raw material is smaller, the droplet generation speed is higher, the reaction raw material is approximately dispersed in the micro-reaction module 17 and the reaction channel 16 of the first reaction section 18, the droplet size of the reaction raw material is larger than the characteristic size of the reaction channel 16, under the shearing action of the wall of the reaction channel 16 facing the droplets, a plurality of relatively independent reaction raw material liquid columns are formed in the reaction channel 16 and the micro-reaction module 17, the chaotic flow formed by transverse flow and longitudinal flow between the reaction raw material liquid columns is generated simultaneously, meanwhile, the inner circulation flow is generated in the reaction raw material liquid columns, the combined action of the chaotic flow and the inner circulation flow reduces the boundary layer thickness and the molecular diffusion distance of the reaction raw material liquid columns, the contact area and the interface update speed of the reaction raw material liquid columns are increased, and the mass transfer efficiency of the reaction raw material is enhanced, and therefore the rapid mixing and rapid mass transfer between the reaction raw materials are realized in the first reaction section 18.
As shown in fig. 4, the channel spacing in the second reaction section 19 is the largest, in the second reaction section 19, the reaction raw materials mainly adopt stratified flow, the average diameter of droplets of the reaction raw materials is larger, the droplet generation speed is slower, the reaction raw materials are continuously the same in the micro-reaction module 17 and the reaction channel 16 of the second reaction section 19, meanwhile, the reaction liquid raw materials do not have internal circulation flow in the second reaction section 19, the mass transfer mode between the reaction liquid raw materials mainly adopts molecular diffusion, the molecular-grade close contact with the catalyst filler 21 in the second reaction section 19 can be realized, and the contact area between the reaction raw materials and the catalyst is increased; in addition, the flow rate of the reaction raw materials in the second reaction section 19 is the slowest, so that the contact time of the reaction raw materials and the catalyst filler 21 can be prolonged to the greatest extent, thereby ensuring that the catalytic reaction is completely carried out, and greatly improving the reaction rate, so that the whole reaction raw materials can be fully reacted.
As shown in fig. 4, the channel spacing in the third reaction section 20 is between the first reaction section 18 and the second reaction section 19, and the effect of the third reaction section 20 is to hydrolyze the reaction solution obtained by the reaction in the second reaction section 19 at a high temperature, so that the temperature condition required by the hydrolysis reaction needs to be satisfied, but the temperature required by the hydrolysis reaction is higher than the temperature required by the catalytic reaction in the second reaction section 19, the temperature of the catalytic reaction in the second reaction section 19 is controlled between 70 ℃ and 80 ℃, the temperature of the hydrolysis reaction in the third reaction section 20 needs to be 100 ℃ to 110 ℃, but the temperatures of the heat exchange media flowing in the top layer 1 and the bottom layer 3 are consistent everywhere, and the temperature of the third reaction section 20 cannot be independently controlled by independently controlling the temperature of the heat exchange media at different positions of the heat exchange channels, so that the heat transfer efficiency and the heat preservation effect of the third reaction section 20 can be improved only on the premise that the temperature of the heat exchange media is kept unchanged, so that the reaction solution in the third reaction section 20 can obtain more heat to reach the temperature condition of the hydrolysis reaction. Therefore, the invention controls the flowing state of the reaction liquid in the third reaction section 20 by adjusting the channel spacing of the third reaction section 20, so that the reaction liquid alternately generates layering flow and liquid drop flow when passing between the micro-reaction module 17 and the reaction channel 16, the duty ratio of the two flowing states is kept balanced, and relative movement is generated between different flow lines on the flowing interface under the combined action of the two flowing states, thereby improving the contact area between the reaction liquid, reducing the temperature boundary layer thickness of the reaction liquid, shortening the heat exchange path of the heat exchange medium of the top layer 1 and the bottom layer 3, enabling the reaction liquid in the third reaction section 20 to receive more heat of the heat exchange medium, and compared with the first reaction section 18 and the second reaction section 19, the reaction temperature in the third reaction section 20 is greatly improved; in addition, a small amount of catalyst filler 21 is further arranged in the third reaction section 20, so that the catalytic effect can be continuously exerted on one hand, more importantly, a small amount of catalyst filler 21 dispersed in the third reaction section 20 can play a role of a static mixing piece, when the reaction liquid flows through the catalyst filler 21, the catalyst filler 21 can generate a cutting effect on the reaction liquid, so that the reaction liquid rearranges and recombines, the effect increases the contact area between the reaction liquids, and meanwhile, the updating iteration between the inside and the surface layer of the reaction liquid is accelerated along with the stretching, deformation and folding effects on the microelements of the reaction liquid, so that the temperature of each part of the reaction liquid is uniform and stable in a short time, and the progress of the hydrolysis reaction is accelerated.
In some alternative embodiments, as shown in FIG. 4, the catalyst loading in the first reaction zone 18 is equal throughout, the catalyst loading in the second reaction zone 19 is equal throughout, the catalyst loading in the third reaction zone 20 is equal throughout, and the catalyst loading in the first reaction zone 18 < the catalyst loading in the third reaction zone 20 < the catalyst loading in the second reaction zone 19.
Specifically, as shown in fig. 4, the catalyst is not filled in the first reaction section 18, the catalyst filling amount in the second reaction section 19 is 70 to 80wt% of the total catalyst filling amount, and the catalyst filling amount in the third reaction section 20 is 20 to 30wt% of the total catalyst filling amount.
In another embodiment, the invention provides a method for producing tartaric acid by adopting the microchannel reaction device provided by the embodiment, which specifically comprises the following steps:
(1) Filling a tungstic acid catalyst in the groove structure, wherein the mass ratio of the tungstic acid catalyst to maleic anhydride is (0.005-0.01): 1; introducing heat exchange medium at 100-120 ℃ into the first heat exchange channel 8 and the second heat exchange channel 11 to heat the reaction layer 2;
(2) Injecting deionized water, maleic anhydride and 25-30wt% of hydrogen peroxide solution into the micro-channel reaction device through different feed channels respectively, wherein the mass ratio of the deionized water to the maleic anhydride to the hydrogen peroxide solution is 1 (0.9-1) (1.4-1.6); the reaction raw materials are mixed in the reaction channel 16 and the micro-reaction module 17, and when flowing through the tungstic acid catalyst filling layer, the reaction takes place under the action of the tungstic acid catalyst to generate epoxy succinic acid solution;
(3) And (3) discharging the epoxy succinic acid solution from a micro-channel reaction device through a discharging channel 7, heating the epoxy succinic acid solution to 105-115 ℃ for hydrolysis reaction for 3-4h, then cooling to 5-10 ℃ for self-crystallization, finally carrying out suction filtration to obtain crystals, and drying the crystals to obtain the tartaric acid.
Example 1
The present embodiment provides a microchannel reactor for producing tartaric acid, which is based on the above embodiment, wherein the length of the first reaction section 18 in the y direction is 15% of the total length of the reaction channel 16, the length of the second reaction section 19 in the y direction is 80% of the total length of the reaction channel 16, and the length of the third reaction section 20 in the y direction is 5% of the total length of the reaction channel 16.
The ratio of the channel spacing of the first reaction section 18, the second reaction section 19 and the third reaction section 20 is 1:1.5:1.3. The catalyst was not filled in the first reaction zone 18, the catalyst filling amount in the second reaction zone 19 was 70wt% of the total catalyst filling amount, and the catalyst filling amount in the third reaction zone 20 was 30wt% of the total catalyst filling amount.
The embodiment also provides a method for producing tartaric acid by adopting the microchannel reaction device, which comprises the following steps:
(1) Filling a tungstic acid catalyst in the groove structure, wherein the mass ratio of the tungstic acid catalyst to maleic anhydride is 0.005:1; introducing heat exchange medium at 100 ℃ into the first heat exchange channel 8 and the second heat exchange channel 11 to heat the reaction layer 2;
(2) Injecting deionized water, maleic anhydride and 25wt% hydrogen peroxide solution into the micro-channel reaction device through different feed channels respectively, wherein the mass ratio of the deionized water to the maleic anhydride to the hydrogen peroxide solution is 1:0.9:1.4; the reaction raw materials are mixed in the reaction channel 16 and the micro-reaction module 17, and when flowing through the tungstic acid catalyst filling layer, the reaction takes place under the action of the tungstic acid catalyst to generate epoxy succinic acid solution;
(3) And (3) discharging the epoxy succinic acid solution from a micro-channel reaction device through a discharging channel 7, heating the epoxy succinic acid solution to 105 ℃ for hydrolysis reaction for 4 hours, then cooling to 5 ℃ for self-crystallization, and finally carrying out suction filtration to obtain crystals, wherein the crystals are dried to obtain the tartaric acid.
Example 2
The present embodiment provides a microchannel reactor for producing tartaric acid, which is based on the above embodiment, wherein the length of the first reaction section 18 in the y direction is 18% of the total length of the reaction channel 16, the length of the second reaction section 19 in the y direction is 75% of the total length of the reaction channel 16, and the length of the third reaction section 20 in the y direction is 7% of the total length of the reaction channel 16.
The ratio of the channel spacing of the first reaction section 18, the second reaction section 19 and the third reaction section 20 is 1:1.6:1.4. The catalyst was not filled in the first reaction zone 18, the catalyst filling amount in the second reaction zone 19 was 72wt% of the total catalyst filling amount, and the catalyst filling amount in the third reaction zone 20 was 28wt% of the total catalyst filling amount.
The embodiment also provides a method for producing tartaric acid by adopting the microchannel reaction device, which comprises the following steps:
(1) Filling a tungstic acid catalyst in the groove structure, wherein the mass ratio of the tungstic acid catalyst to maleic anhydride is 0.006:1; introducing heat exchange medium at 105 ℃ into the first heat exchange channel 8 and the second heat exchange channel 11 to heat the reaction layer 2;
(2) Injecting deionized water, maleic anhydride and 26wt% of hydrogen peroxide solution into the micro-channel reaction device through different feed channels respectively, wherein the mass ratio of the deionized water to the maleic anhydride to the hydrogen peroxide solution is 1:0.92:1.5; the reaction raw materials are mixed in the reaction channel 16 and the micro-reaction module 17, and when flowing through the tungstic acid catalyst filling layer, the reaction takes place under the action of the tungstic acid catalyst to generate epoxy succinic acid solution;
(3) And (3) discharging the epoxy succinic acid solution from a micro-channel reaction device through a discharging channel 7, heating the epoxy succinic acid solution to 108 ℃ for hydrolysis reaction for 3.8 hours, then cooling to 6 ℃ for self-crystallization, and finally carrying out suction filtration to obtain crystals, wherein the crystals are dried to obtain the tartaric acid.
Example 3
The present embodiment provides a micro-channel reaction device for producing tartaric acid, which is based on the above specific embodiment, wherein the length of the first reaction section 18 in the y direction is 20% of the total length of the reaction channel 16, the length of the second reaction section 19 in the y direction is 70% of the total length of the reaction channel 16, and the length of the third reaction section 20 in the y direction is 10% of the total length of the reaction channel 16.
The ratio of the channel spacing of the first reaction section 18, the second reaction section 19 and the third reaction section 20 is 1:1.7:1.4. The catalyst was not filled in the first reaction zone 18, the catalyst filling amount in the second reaction zone 19 was 75wt% of the total catalyst filling amount, and the catalyst filling amount in the third reaction zone 20 was 25wt% of the total catalyst filling amount.
The embodiment also provides a method for producing tartaric acid by adopting the microchannel reaction device, which comprises the following steps:
(1) Filling a tungstic acid catalyst in the groove structure, wherein the mass ratio of the tungstic acid catalyst to maleic anhydride is 0.007:1; a heat exchange medium at 110 ℃ is introduced into the first heat exchange channel 8 and the second heat exchange channel 11 to heat the reaction layer 2;
(2) Injecting deionized water, maleic anhydride and 27wt% hydrogen peroxide solution into the micro-channel reaction device through different feed channels respectively, wherein the mass ratio of the deionized water to the maleic anhydride to the hydrogen peroxide solution is 1:0.95:1.45; the reaction raw materials are mixed in the reaction channel 16 and the micro-reaction module 17, and when flowing through the tungstic acid catalyst filling layer, the reaction takes place under the action of the tungstic acid catalyst to generate epoxy succinic acid solution;
(3) And (3) discharging the epoxy succinic acid solution from a micro-channel reaction device through a discharging channel 7, heating the epoxy succinic acid solution to 110 ℃ for hydrolysis reaction for 3.5 hours, then cooling to 7 ℃ for self-crystallization, and finally carrying out suction filtration to obtain crystals, wherein the crystals are dried to obtain the tartaric acid.
Example 4
The present embodiment provides a microchannel reactor for producing tartaric acid, which is based on the above embodiment, wherein the length of the first reaction section 18 in the y direction is 25% of the total length of the reaction channel 16, the length of the second reaction section 19 in the y direction is 70% of the total length of the reaction channel 16, and the length of the third reaction section 20 in the y direction is 5% of the total length of the reaction channel 16.
The ratio of the channel spacing of the first reaction section 18, the second reaction section 19 and the third reaction section 20 is 1:1.8:1.5. The catalyst was not filled in the first reaction zone 18, the catalyst filling amount in the second reaction zone 19 was 78wt% of the total catalyst filling amount, and the catalyst filling amount in the third reaction zone 20 was 22wt% of the total catalyst filling amount.
The embodiment also provides a method for producing tartaric acid by adopting the microchannel reaction device, which comprises the following steps:
(1) Filling a tungstic acid catalyst in the groove structure, wherein the mass ratio of the tungstic acid catalyst to maleic anhydride is 0.008:1; introducing 115 ℃ heat exchange medium into the first heat exchange channel 8 and the second heat exchange channel 11 to heat the reaction layer 2;
(2) Injecting deionized water, maleic anhydride and 28wt% of hydrogen peroxide solution into the micro-channel reaction device through different feed channels respectively, wherein the mass ratio of the deionized water to the maleic anhydride to the hydrogen peroxide solution is 1:0.98:1.5; the reaction raw materials are mixed in the reaction channel 16 and the micro-reaction module 17, and when flowing through the tungstic acid catalyst filling layer, the reaction takes place under the action of the tungstic acid catalyst to generate epoxy succinic acid solution;
(3) And (3) discharging the epoxy succinic acid solution from a micro-channel reaction device through a discharging channel 7, heating the epoxy succinic acid solution to 112 ℃ for hydrolysis reaction for 3.2 hours, then cooling to 8 ℃ for self-crystallization, and finally carrying out suction filtration to obtain crystals, wherein the crystals are dried to obtain the tartaric acid.
Example 5
The present embodiment provides a micro-channel reaction device for producing tartaric acid, which is based on the above specific embodiment, wherein the length of the first reaction section 18 in the y direction is 30% of the total length of the reaction channel 16, the length of the second reaction section 19 in the y direction is 60% of the total length of the reaction channel 16, and the length of the third reaction section 20 in the y direction is 10% of the total length of the reaction channel 16.
The ratio of the channel spacing of the first reaction section 18, the second reaction section 19 and the third reaction section 20 is 1:2:1.6. The catalyst was not filled in the first reaction zone 18, the catalyst filling amount in the second reaction zone 19 was 80wt% of the total catalyst filling amount, and the catalyst filling amount in the third reaction zone 20 was 20wt% of the total catalyst filling amount.
The embodiment also provides a method for producing tartaric acid by adopting the microchannel reaction device, which comprises the following steps:
(1) Filling a tungstic acid catalyst in the groove structure, wherein the mass ratio of the tungstic acid catalyst to maleic anhydride is 0.01:1; introducing 120 ℃ heat exchange medium into the first heat exchange channel 8 and the second heat exchange channel 11 to heat the reaction layer 2;
(2) Injecting deionized water, maleic anhydride and 30wt% hydrogen peroxide solution into the micro-channel reaction device through different feed channels respectively, wherein the mass ratio of the deionized water to the maleic anhydride to the hydrogen peroxide solution is 1:1:1.6; the reaction raw materials are mixed in the reaction channel 16 and the micro-reaction module 17, and when flowing through the tungstic acid catalyst filling layer, the reaction takes place under the action of the tungstic acid catalyst to generate epoxy succinic acid solution;
(3) And (3) discharging the epoxy succinic acid solution from a micro-channel reaction device through a discharging channel 7, heating the epoxy succinic acid solution to 115 ℃ for hydrolysis reaction for 3 hours, then cooling to 10 ℃ for self-crystallization, and finally carrying out suction filtration to obtain crystals, wherein the crystals are dried to obtain the tartaric acid.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.
Claims (10)
1. The microchannel reaction device for producing tartaric acid is characterized by comprising a top layer, a reaction layer and a bottom layer which are sequentially laminated and detachably fixed;
the inside of the top layer is provided with a first heat exchange channel which is relatively closed, and the inside of the bottom layer is provided with a second heat exchange channel which is relatively closed; a first heat exchange medium inlet and a first heat exchange medium outlet which are communicated with the first heat exchange channel are formed in the side edge of the top layer; a second heat exchange medium inlet and a second heat exchange medium outlet which are connected with the second heat exchange channel are formed in the side edge of the bottom layer;
three feeding channels and one discharging channel are formed in the top surface of the top layer, and the feeding channels and the discharging channels avoid the first heat exchange channel and are communicated with the reaction layer;
the reaction layer comprises a plurality of mutually independent micro-reaction modules which are arranged in a matrix, wherein each micro-reaction module is of a Z-shaped convex structure, a continuous folded line-shaped groove structure is formed between every two adjacent micro-reaction modules, and the groove structures are mutually communicated to form a reaction channel;
the side of the micro-reaction module is provided with at least two open holes, the convex structures are communicated with the adjacent groove structures through the open holes so as to form a continuous flow path of reaction liquid, and the reaction liquid flows into the groove structures from the convex structures or flows into the convex structures from the groove structures through the open holes;
The inside of the groove structure is filled with a catalyst.
2. The microchannel reactor according to claim 1, wherein the microchannel reactor has a rectangular structure with a long side and a wide side, the wide side of the microchannel reactor being defined as the x-direction, the long side of the microchannel reactor being defined as the y-direction, and a plurality of the microreaction modules being arranged at equal intervals along the x-direction and the y-direction, respectively;
the two ends of the reaction layer in the y direction are also respectively provided with a liquid inlet tank and a liquid outlet tank, and the liquid inlet tank and the liquid outlet tank are respectively communicated with the two ends of the reaction channel in the y direction;
the three feeding channels are a first feeding channel, a second feeding channel and a third feeding channel which are arranged along the x direction respectively, the feeding ends of the first feeding channel, the second feeding channel and the third feeding channel are positioned on the surface of the top layer, the outlet ends of the first feeding channel, the second feeding channel and the third feeding channel are positioned in the reaction layer and are communicated with the liquid inlet tank, deionized water, maleic anhydride and hydrogen peroxide enter the liquid inlet tank through the first feeding channel, the second feeding channel and the third feeding channel respectively, and flow into the reaction channel after being mixed in the liquid inlet tank;
The inlet end of the discharging channel is communicated with the liquid outlet pool, and reaction products obtained by the reaction in the reaction channel are collected into the liquid outlet pool and discharged through the discharging channel;
the outlet end of the discharging channel is connected with a liquid collecting bottle; the liquid collecting bottle is externally connected with a vacuumizing device, and the vacuumizing device is used for vacuumizing the liquid collecting bottle so as to suck reaction products in the liquid outlet pool into the liquid collecting bottle through the discharging channel; the liquid collecting bottle is further provided with a pressure regulating valve and a vacuum gauge, the pressure regulating valve is used for regulating negative pressure in the liquid collecting bottle, and the vacuum gauge is used for monitoring vacuum degree in the liquid collecting bottle.
3. The microchannel reactor according to claim 1, wherein the microreaction module is divided into a first lateral projection, a longitudinal projection and a second lateral projection which are sequentially communicated, wherein the first lateral projection and the second lateral projection are parallel to an x-direction and the longitudinal projection is parallel to a y-direction;
the two ends of the first transverse bulge in the x direction are a first transverse end and a second transverse end respectively, the two ends of the longitudinal bulge in the y direction are a first longitudinal end and a second longitudinal end respectively, and the two ends of the second transverse bulge in the x direction are a third transverse end and a fourth transverse end respectively;
The first transverse end is provided with a first opening, the second transverse end is vertically butted with the first longitudinal end, the second longitudinal end is vertically butted with the third transverse end, and the fourth transverse end is provided with a second opening;
the reaction raw materials enter the micro-reaction module through the first opening, and flow out from the second opening along the first transverse bulge, the longitudinal bulge and the second transverse bulge in sequence; or the micro-reaction module enters from the second opening, and flows out from the first opening along the second transverse bulge, the longitudinal bulge and the first transverse bulge in sequence.
4. The microchannel reactor according to claim 1, wherein the first heat exchange channel and the second heat exchange channel are both serpentine in structure, and the heat exchange medium flows from one end to the other end in the x direction after entering the first heat exchange channel, and returns back at the other end, and is serpentine in shape in the y direction; after the heat exchange medium enters the second heat exchange channel, one end of the heat exchange medium flows to the other end along the y direction, and the heat exchange medium returns back to the other end and is pushed in a serpentine manner along the x direction;
the first heat exchange medium inlet and the first heat exchange medium outlet are positioned on the same side edge of the top layer in the y direction or respectively positioned on two opposite side edges of the top layer in the y direction; the second heat exchange medium inlet and the second heat exchange medium outlet are positioned on the same side of the top layer in the x direction or respectively positioned on two opposite sides of the top layer in the x direction.
5. The microchannel reactor according to claim 1, wherein the first heat exchange channel and the second heat exchange channel are both serpentine in structure, and the heat exchange medium flows from one end to the other end in the y direction after entering the first heat exchange channel, and returns back at the other end, and is serpentine in shape in the x direction; after the heat exchange medium enters the second heat exchange channel, one end of the heat exchange medium flows to the other end along the x direction, and the heat exchange medium returns back to the other end and is pushed in a serpentine manner along the y direction;
the first heat exchange medium inlet and the first heat exchange medium outlet are positioned on the same side of the top layer in the x direction or respectively positioned on two opposite sides of the top layer in the x direction; the second heat exchange medium inlet and the second heat exchange medium outlet are positioned on the same side of the top layer in the y direction or respectively positioned on two opposite sides of the top layer in the y direction.
6. The microchannel reactor according to claim 1, wherein the reaction channel is divided into a first reaction section, a second reaction section and a third reaction section having different lengths in the y direction, the length of the third reaction section in the y direction < the length of the first reaction section in the y direction < the length of the second reaction section in the y direction;
The length of the first reaction section in the y direction is 15-30% of the total length of the reaction channel, the length of the second reaction section in the y direction is 60-80% of the total length of the reaction channel, and the length of the third reaction section in the y direction is 5-10% of the total length of the reaction channel.
7. The micro-channel reaction apparatus according to claim 6, wherein a distance between longitudinal protrusions of two adjacent micro-reaction modules in the x-direction is a channel pitch;
the channel spacing in the first reaction section is the same, the channel spacing in the second reaction section is the same, the channel spacing in the first reaction section is less than the channel spacing in the third reaction section is less than the channel spacing in the second reaction section;
the ratio of the channel spacing of the first reaction section, the second reaction section and the third reaction section is 1 (1.5-2) to 1.3-1.6.
8. The microchannel reactor according to claim 6, wherein the catalyst loading in the first reaction zone is equal everywhere, the catalyst loading in the second reaction zone is equal everywhere, the catalyst loading in the third reaction zone is equal everywhere, and the catalyst loading in the first reaction zone < the catalyst loading in the third reaction zone < the catalyst loading in the second reaction zone;
The catalyst is not filled in the first reaction section, the catalyst filling amount in the second reaction section is 70-80wt% of the total catalyst filling amount, and the catalyst filling amount in the third reaction section is 20-30wt% of the total catalyst filling amount.
9. A process for the preparation of tartaric acid, characterized in that it is carried out in a microchannel reaction device according to any one of claims 1 to 8, comprising:
filling a tungstic acid catalyst in the groove structure, and introducing heat exchange media into the first heat exchange channel and the second heat exchange channel to heat the reaction layer;
(II) respectively injecting deionized water, maleic anhydride and hydrogen peroxide solution into the micro-channel reaction device through different feed channels, mixing reaction raw materials in the reaction channels and the micro-reaction module, and reacting under the action of a tungstic acid catalyst to generate epoxy succinic acid solution when flowing through a tungstic acid catalyst filling layer;
and (III) discharging the epoxy succinic acid solution from a micro-channel reaction device through a discharging channel, heating and hydrolyzing the epoxy succinic acid solution, then cooling and self-crystallizing, finally carrying out suction filtration to obtain crystals, and drying the crystals to obtain the tartaric acid.
10. The process according to claim 9, wherein in step (i), the temperature of the heat exchange medium is 100-120 ℃;
the mass ratio of the tungstic acid catalyst to the maleic anhydride is (0.005-0.01): 1;
in the step (II), the mass ratio of the deionized water to the maleic anhydride to the hydrogen peroxide solution is 1 (0.9-1): 1.4-1.6;
the mass fraction of the hydrogen peroxide solution is 25-30wt%;
in the step (III), the reaction temperature of the heated hydrolysis is 105-115 ℃;
the reaction time of the heating hydrolysis is 3-4 hours;
the temperature of the cooling is 5-10 ℃.
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