CN208944071U - A kind of anti-settling based on 3D printing declines reactor and synthesis system - Google Patents

Abstract

The utility model relates to synthesis reactor, proposing that a kind of anti-settling based on 3D printing declines reactor, comprising: the channel of the microreactor is shape of the included curvature along coiled coil, meanwhile, the entire microreactor is the shape of coiled coil.The utility model also proposes a kind of synthesis system, it include: reaction unit (7), for accessing at least two fluids, two kinds of fluids are in the raw reaction of the interior hybrid concurrency of reaction unit (7), reaction unit (7) includes that the mixer (71) being linked in sequence and 3D printing decline reactor (72), wherein the channel of the microreactor is shape of the included curvature along coiled coil, meanwhile the entire microreactor is the shape of coiled coil.The utility model can generate the product quality and yield of needs in a relatively short period of time, increase the conversion ratio of product, and energy-saving effect is obvious.

Description

A kind of anti-settling based on 3D printing declines reactor and synthesis system

Technical field

The utility model relates to synthesis reactor, decline reaction more particularly, to a kind of anti-settling based on 3D printing Device and synthesis system.

Background technique

2,5- chlorophenesic acids are more important organic synthesis intermediate and pesticide intermediate, can be used for synthesizing 3,6- dichloro Salicylic acid generates ester etc. with acetic acid condensation.It is mainly used for nitrogen fertilizer potentiating agent, manufacture herbicide dicamba, leather fungicide and DP Mould inhibitor etc..

2,5- chlorophenesic acid is produced so that 1,2,4- trichloro-benzenes is raw material, mainly has non-pressure process and pressurization two different Method.But non-pressure process is because ethylene glycol dosage is big, difficult recycling, unstable product quality and be rejected, pressurization becomes usually used Technique.Its technique are as follows: using trichloro-benzenes, solid caustic soda and methanol as raw material, high temperature (190 DEG C) high pressure (4.3MPa) hydrolyzes 4h, passes through Filter, acidification, extraction, rectifying, obtain 2, the 5- chlorophenesic acid crude product of 96% or more content, yield 90%~93%.Pass through addition Urea carries out substep crystallization, and the mixture of 2,5- chlorophenesic acid, 2,4- chlorophenesic acid after separation reaction obtains 2,5- dichloro-benzenes The urea adduct of phenol, then hydrolyze and obtain 2,5- chlorophenesic acid.

Existing 2,5- chlorophenesic acid is produced with reaction kettle, and in process of production, the reaction time is too long, reaction Process is not easy to control, and the energy consumption of reaction kettle is very high.The synthesis path of reaction kettle there is also problems, the reaction time is long, Each component concentration distribution is uneven, operational safety is poor, overhead time is long, and reaction temperature control is difficult, especially reacts When heat release is violent, while temperature is unevenly distributed, and is also easy to cause by-product height.

Utility model content

For the problems in background technique, the purpose of this utility model is to provide the 2,5- of a kind of rapid synthesis high-purity Chlorophenesic acid, at the same during reaction reduce side reaction generation, be precisely controlled reaction process, improve the safety of production Property.

The technology path of the utility model is to use microreactor.Microreactor is that a kind of duct type continuously flowed is anti- Answer device.It includes mixer, heat exchanger required for chemical unit, reactor, controller etc., and still, line size is much Less than conventional tube reactor.It is to be formed in parallel inside microreactor by many micro-pipes, has great specific surface area, thus bring Basic advantage be great heat exchange efficiency and mixing efficiency.Reaction temperature and reaction mass can accurately be controlled by accurate proportion Instantaneous mixing.These are all to improve yield, selectivity, safety and the key factor for improving product quality, microreactor The purpose of realization expanding production that can be relatively easy, there is very wide application prospect in the following chemical field.

Decline reactor the utility model proposes a kind of anti-settling based on 3D printing, the channel of the microreactor be from With curvature along the shape of coiled coil, meanwhile, the entire microreactor is the shape of coiled coil.

Optionally, heat exchange fluid jacket is enclosed with outside the channel of the microreactor, the microreactor includes sequence The bringing-up section and condensation segment of connection, heating fluid are flowed through out of bringing-up section casing, and cooling fluid is flowed out of condensation segment casing It crosses.

Optionally, heating fluid is flowed into from some section of bringing-up section lateral ends, is flowed out at bringing-up section inner opposite end； Cooling fluid is flowed into from some section of the other end of lateral ends of condensation segment, is flowed out at condensation segment inner opposite end.Optionally, Opening is provided on casing, redundancy is inserted into ultrasonic transmitter in casing.

The utility model also proposes a kind of to decline the synthesis system of reactor including 3D printing, comprising: reaction unit is used for At least two fluids, the raw reaction of two kinds of fluids hybrid concurrency in reaction unit are accessed, reaction unit includes the mixed of sequential connection Clutch and 3D printing decline reactor, wherein the channel of the microreactor is shape of the included curvature along coiled coil, together When, the entire microreactor is the shape of coiled coil.

Optionally, reaction unit connection is there are two branch, and a branch includes: the first container, first-class of sequential connection Measure metering pump and first micro- heat exchanger；Another branch includes: the second container of sequential connection, second flow metering pump and second Micro- heat exchanger.

Optionally, mixer is five-layer structure, and first layer structure is identical as layer 5 structure, second layer structure with the 4th layer Structure is identical, wherein is provided with aperture in first layer structure；Diversion cavity and groove are provided in second layer structure, under diversion cavity Trip is provided with multiple microchannels, leads to the groove；Groove is provided in third layer structure, in second layer structure and third layer structure Groove overlapping；Mixing chamber is formed after the five-layer structure superposition.

Optionally, there is cavity on the bottom surface of first layer structure, the aperture is in cavity, the cavity and the diversion cavity It is corresponding.

Optionally, heat exchange fluid jacket is enclosed with outside the channel of the microreactor, the microreactor includes sequence The bringing-up section and condensation segment of connection, heating fluid are flowed through out of bringing-up section casing, and cooling fluid is flowed out of condensation segment casing It crosses；Inserted with ultrasonic transmitter in the casing of the pico- reactor.Optionally, the synthesis system further include: collect Container is connected to after reaction unit；For the counterbalance valve of boosting, the counterbalance valve is mounted at the top of collection vessel.

The utility model has the following beneficial effects:

The utility model patent passes through continuously amplification effect using current novel micro-mixer, micro- heat exchanger, microreactor The product quality and yield that generate needs in a relatively short period of time should be reached.

Relative to traditional chemical industry production model, the utility model increases the conversion ratio of product, and energy-saving effect is obvious, anti- The stage is answered, the crystal form for controlling and monitoring reaction is can be very good, reduces production cost.It is well sold and in short supply that the utility model is well suited for market Stable product, because early investment is very big, but yield is high, effect stability.

The utility model reduces the time required for reaction using microreactor, realizes within the shorter residence time Secondly the Efficient Conversion rate of 2,5- chlorophenesic acids has the generation of NaCl crystal in the present reaction, prevent NaCl heavy using ultrasonic wave Drop, the sedimentation of particle in microchannel is prevented by the design to microreactor, makes to react continuous-stable progress.

Detailed description of the invention

Fig. 1 is the structure principle chart of the synthesis system of the utility model.

Fig. 2 is the first layer of mixer and the perspective view of layer 5.

Fig. 3 is the first layer of mixer and the top view of layer 5.

Fig. 4 is the second layer of mixer and the perspective view of four-layer structure.

Fig. 5 is the second layer of mixer and the top view of four-layer structure.

Fig. 6 is the perspective view of the third layer structure of mixer.

Fig. 7 is the perspective view of the depression angle of mixer.

Fig. 8 is the perspective view for looking up angle of mixer.

Fig. 9 is the perspective view of microreactor.

Figure 10 is the perspective view of microreactor.

Figure 11 is the sectional view of microreactor.

Appended drawing reference

The first container 1, second container 2, first flow metering pump 3,4, first micro- heat exchanger 5 of second flow metering pump, the Two micro- heat exchangers 6, reaction unit 7, ultrasonic transmitter 8, counterbalance valve 9, valve 10, outlet 11, collection vessel 12, mixer 71, microreactor 72, first layer structure L1, second layer structure L2, third layer structure L3, four-layer structure L4, layer 5 structure L5, aperture L11, cavity L12, diversion cavity L21, microchannel L22, groove L23, groove L31.

Specific embodiment

The embodiments of the present invention is described with reference to the accompanying drawings, wherein the identical appended drawing reference table of identical component Show.In the absence of conflict, the technical characteristic in following embodiment and embodiment can be combined with each other.

The utility model is described so that 1,2,4- trichloro-benzenes is object below, i.e., it is 1,2,4- trichloro-benzenes and sodium hydroxide is molten In methanol.But the utility model is without being limited thereto, other organic synthesis intermediates and pesticide intermediate also can be applied to The utility model.

As shown in Figure 1, the system of the utility model includes reaction unit 7, reaction unit 7 is at least connected with two branches, uses In accessing two kinds of fluids, two kinds of fluids hybrid concurrency in reaction unit 7 is raw to react.First branch includes: sequential connection The first container 1, first flow metering 3, first micro- heat exchanger 5 of pump.The first container 1 is for storing liquid, first flow metering pump 3 For measuring the amount of liquid flowed through, first micro- heat exchanger 5 can also freeze for heating to the liquid flowed through.Second Branch includes: the second container 2 of sequential connection, second flow metering 4, second micro- heat exchanger 6 of pump.Second container 2 is for storing Liquid, second flow metering pump 4 is for measuring the amount of liquid flowed through, and second micro- heat exchanger 6 is for adding the liquid flowed through Heat can also freeze.

Reaction unit 7 includes the mixer 71 and microreactor 72 being linked in sequence, and mixer 71 is (preceding before reactor 72 After refer to fluid flow direction).Flowing out the liquid of first micro- heat exchanger 5 and second micro- heat exchanger 6, to be introduced into mixer 71 mixed It closes, then flows into microreactor 72 and reacted.

In one embodiment, what is stored in the first container 1 is 26% trichlorine benzyl alcohol solution, is measured and is pumped by first flow 3 control its flow, and trichlorine benzyl alcohol solution is heated via the first micro- heat exchanger 5, the outlet of first micro- heat exchanger 5 via pipeline with Mixer 71 connects.What is stored in second container 2 is 20% sodium hydrate methanol solution, controls it by second flow metering pump 4 Flow, sodium hydrate methanol solution are heated via second micro- heat exchanger 6, and the outlet of second micro- heat exchanger 6 also via pipeline and mixes Clutch 71 connects.

For the trichlorine benzyl alcohol solution that concentration is 26% by first flow metering pump 1,20% sodium hydrate methanol solution is logical Cross second flow metering pump 2.20% sodium hydrate methanol solution and concentration are 26% trichlorine benzyl alcohol solution before mixer 71 First micro- heat exchanger 5, be heated to 150-180 degrees Celsius at second micro- heat exchanger 6, the liquid after heating is mixed in mixer 71 It closes, then mixed liquid flows into reactor 72.The temperature of reactor 72 is maintained at 190-220 degrees Celsius.1-2-4 trichloro-benzenes Start to participate in reaction at 180 degrees Celsius with the methanol solution of NaOH, at 210 degrees Celsius, reaction efficiency height is higher while micro- The back pressure of reactor is controlled in 50bar.

Mixer 71 is a five-layer structure, and Fig. 2 shows the first layer of mixer 71 and the perspective view of layer 5, Fig. 3 Show that the first layer of mixer 71 and the top view of layer 5, Fig. 4 show the second layer and four-layer structure of mixer 71 Perspective view, Fig. 5 shows that the perspective view of the third layer structure of mixer 71, Fig. 6 show the third layer structure of mixer 71 Top view.Fig. 7 shows the perspective view of the depression angle of mixer 71, and what Fig. 8 showed mixer 71 looks up the vertical of angle Body figure.

It is provided with aperture L11 on first layer structure L1, has rectangular cavity L12 on bottom surface, the aperture is in cavity.First The aperture L11 of layer structure is the import of one of fluid, and fluid is flowed into from aperture L11, into cavity L12.Preferably, aperture L11 is located at the center of cavity L12.

Be provided on the second layer structure L2 diversion cavity L21 (can be fan-shaped or trapezoidal), diversion cavity L21 be it is inclined, The downstream (at trapezoidal short side or fan handle) of diversion cavity is provided with multiple microchannel L22 (such as 10, having a size of 300um).The Groove L23 is provided on two-layer structure L2, microchannel L22 leads to groove L23.The size of diversion cavity L21 is matched with cavity L12, The liquid flowed into will not be flowed out from the second layer edge structure L2, but enter the mixed of third layer structure L3 from diversion cavity L21 Chamber is closed to be mixed.

It is provided with groove L31 on third layer structure L3, when superposition, groove L31 is Chong Die with groove L23.When first layer structure L1, When second layer structure L2 and third layer structure L3 are superimposed, the plate of first layer structure L1 can block the upper surface of groove L31.Separately Outside, because four-layer structure L4 is identical as second layer structure L2, layer 5 structure L5 is identical as first layer structure L1.Therefore the 5th Layer structure has been blocked below groove L31, to form mixing chamber.The formation of mixing chamber is the stacking by 5 layers of structure.

Perspective view after whole 5 layers of folded structures is as Figure 7-8, and wherein Fig. 7 is perspective view, and Fig. 8 is perspective view.

A kind of liquid enters second layer structure from first layer structure, and fluid first in the diversion cavity of second layer structure, then exists The downstream of diversion cavity is dispersed into the cuboid mixing chamber of third layer by microchannel, and another fluid streams equally pass through layer 5 knot Structure enters the 4th layer, is dispersed into the cuboid mixing chamber of third layer by microchannel by the downstream of the 4th layer of diversion cavity.It is mixed The outlet L32 for closing chamber is connected with microreactor 72.

Fig. 9 shows that the perspective view of microreactor 72, Figure 10 show that the perspective view of microreactor 72, Figure 11 are shown The sectional view of microreactor 72.The channel internal diameter (6mm) of microreactor 72 is smaller than the internal diameter of the outlet L32 of mixer 71, stream Speed is improved, and reactor, at specific shape, reaches using 3D printing technological design and increases stopping for reaction in unit length The production rate for staying the time, improving target product.

The channel of microreactor 72 is shape of the included curvature along coiled coil.Fig. 9 shows whole helical structure, In each section be also with curvature helical structure.The helical form internal diameter G1 to spiral can be 40mm, microreactor 72 it is total Length H1 can be 1m, and the curvature of microchannel meets the flowing requirement of fluid, saved the land used of workshop, and is also able to satisfy life The demand of runoff yield, and do this shape and can also promote the mixing of two kinds of solution during flowing, accelerate the speed of reaction Degree.

Microreactor 72 amplifies (including geometric dimension amplification, superposition amplification in parallel, number of channels increase etc.) by integrated It realizes enlarge-effect, microreactor is made by specific shape by 3D printing technique in commercial process, reaches flow The demand of the residence time of widened effect and reaction.

Preferably, microreactor 72 is two-part structure, and first segment is bringing-up section, and second segment is condensation segment, in Figure 10, Left side half is bringing-up section, and right side half is condensation segment.Bringing-up section is high temperature (such as 200 degree), is to guarantee that reaction is kept It carries out at high temperature.Condensation segment (such as 25 degree water) is in order to which the vapour pressure of neighbourhood administrative system alkane lowers, thus in subsequent gas-liquid In knockout drum, after pressure discharges, methane will not gasify, and guarantee that the NaCl in methane is not precipitated.Preferably, in bringing-up section There is isolation section, between condensation segment to guarantee that two-part heat does not transmit.Because the temperature difference is too big between bringing-up section and condensation segment, It is not heat-insulated to have thermal losses.

It is heat exchange fluid jacket in the casing of the outer layer of microreactor 72.At the suitable place of casing for example in left and right ends and Heat-barrier material G2, G6, G10 is arranged in middle.Referring to Fig.1 1, heat fluid from the entrance G3 in a certain section of casing left end into Enter, flowed along microreactor 72, the outlet G5 outflow at the half close to 72 length of microreactor is carried out suitable with this rule Stream heat exchange.Barrier component G4 is set among outlet G5 and storage G3.It can symmetrically be set according to the left side on the right of microreactor 72 The entrance G9 for setting cooling fluid entrance, in middle, setting cooling fluid exports G7, and resistance is arranged among outlet G7 and storage G9 Every component G8, counterflow heat exchange is carried out with this rule.The internal diameter and wall thickness of casing are to guarantee running according to needing to be adjusted The temperature of bearing requirements in journey, heat exchanging fluid is adjustable, to guarantee for the temperature of microreactor 72 to be heated and kept at Need problem.Tee tube is utilized in inside pipe casing, the outlet of microreactor 72 is connected with extraneous heat exchanger.

Referring again to Fig. 1, the system of the utility model further includes ultrasonic transmitter 8.Ultrasonic transmitter 8 is arranged micro- In the casing of 72 outer layer of reactor.Ultrasonic transmitter 8 can issue ultrasound, accelerate the disturbance of solution by ultrasonic wave, and And energy is provided to solution, the dissolution of accelerating impurity avoids impurity from settling.

Referring again to Fig. 1, the system of the utility model further includes collection vessel 12, and collection vessel 12 is connected to reaction unit 7, the top of collection vessel 12 is provided with counterbalance valve 9, what counterbalance valve 9 was used to boost to reaction system, and controls monitoring reaction Pressure.Outlet 11 is provided on collection vessel 12, reaction product is discharged from outlet 11.Collection vessel bottom is provided with valve 10.

In addition, 1, the NaCl that can be generated in the production reaction process that 2,4- trichloro-benzenes and sodium hydroxide are dissolved in methanol, It is easy sedimentation, if taken no action to, in a short period of time, back pressure can be increased sharply.It can be in the left and right of micro-mixer 72 Ultrasonic transmitter is installed in two sides, accelerates the disturbance of solution by ultrasonic wave, and provide energy to solution, prevents NaCl brilliant Body sedimentation.

By the utility model, it is capable of 2, the 5- chlorophenesic acid of rapid synthesis high-purity, while subtracts during reaction The generation of few side reaction, is precisely controlled reaction process, improves the safety of production.

The structure of microreactor 72 is shape of the included curvature along coiled coil, by configuring suitable internal diameter and flow velocity, It can guarantee to carry away NaCl in product by flow control, be unlikely to settle, also ensure and stop in microreactor The time is stayed, conversion ratio is improved.This is because: 1, channel of reactor spirals using helix as axis, and in unit length, pipeline edge Cheng Zengchang increases residence time of the reactant in reactor, so conversion ratio is improved；2, micro- logical under helical structure Road direction is no longer kept constant, and 0-360 will be presented in the deposition direction of fluid direction of motion and NaCl product, i.e. gravity direction The cyclically-varying of degree, therefore the deposition that NaCl product will be inhibited.This is because: fluid is mainly logical to the carrying campaign of particle Drag force is crossed to realize, drag force direction is consistent with flow direction always.In straight tube microchannel, drag force is vertical with gravity, in weight Component is not generated on power deposition direction；And in this scenario, drag force will generate component on gravity direction, when its component and gravity When reversed, drag force is enough to overcome gravity, therefore NaCl product does not deposit；When drag force component and gravity are in the same direction, NaCl is generated Object accelerates under the leading role of drag force, and fluid carries NaCl high speed and washes away microchannel wall face without stagnating, therefore NaCl Product does not deposit.

The utility model is tested: concentration is 26% trichlorine benzyl alcohol solution and concentration is 20% sodium hydroxide methanol Solution is heated to after 170 degree be sufficiently mixed in micro-mixer again in micro heat exchanger, then reacts in microreactor, Microreactor reaction temperature is maintained at 210 degree, and system back pressure 5MPa, solution residence time 0.5 in microreactor Minute, the conversion ratio 100% of trichloro-benzenes, yield 75%.

This technology route greatly shortens the time of reaction, improves the yield of 2,5- chlorophenesic acid, also effectively controls The generation of the side reaction of reaction, the production model traditional relative to reaction kettle, the utility model greatly improve production process The degree of automation and security performance etc..

Embodiment described above, only the utility model more preferably specific embodiment, those skilled in the art The usual variations and alternatives carried out within the scope of technical solutions of the utility model should all be included in the protection scope of the utility model It is interior.

Claims (10)

1. The reactor 1. a kind of anti-settling based on 3D printing declines, which is characterized in that

   The channel of the microreactor is shape of the included curvature along coiled coil, meanwhile, the entire microreactor is spiral The shape of coiling.
2. 2. microreactor according to claim 1, which is characterized in that

   Heat exchange fluid jacket is enclosed with outside the channel of the microreactor, the microreactor includes the bringing-up section being linked in sequence And condensation segment, heating fluid are flowed through out of bringing-up section casing, cooling fluid is flowed through out of condensation segment casing.
3. 3. microreactor according to claim 2, which is characterized in that

   It heats fluid to flow into from some section of bringing-up section lateral ends, be flowed out at bringing-up section inner opposite end；Cooling fluid from Some section of the other end of the lateral ends of condensation segment flows into, and flows out at condensation segment inner opposite end.
4. 4. microreactor according to claim 2, which is characterized in that

   Opening is provided on casing, redundancy is inserted into ultrasonic transmitter in casing.
5. 5. a kind of synthesis system characterized by comprising

   Reaction unit (7), for accessing at least two fluids, two kinds of fluids are in the raw reaction of the interior hybrid concurrency of reaction unit (7), instead Answering device (7) includes that the mixer (71) being linked in sequence and the 3D printing for anti-settling decline reactor (72),

   Wherein, the channel of the microreactor is shape of the included curvature along coiled coil, meanwhile, the entire microreactor is The shape of coiled coil.
6. 6. synthesis system according to claim 5, which is characterized in that

   There are two branch, a branch includes: the first container (1) of sequential connection, first flow metering for reaction unit (7) connection Pump (3) and first micro- heat exchanger (5)；Another branch includes: the second container (2) of sequential connection, second flow metering pump (4) With second micro- heat exchanger (6).
7. 7. synthesis system according to claim 6, which is characterized in that

   Mixer (71) is five-layer structure, and first layer structure is identical as layer 5 structure, second layer structure and four-layer structure phase Together,

   Wherein, it is provided in first layer structure aperture (L11)；

   Diversion cavity (L21) and groove (L23) are provided in second layer structure, the downstream of diversion cavity (L21) is provided with multiple micro- logical Road (L22) leads to the groove (L23)；

   It is provided in third layer structure groove (L31), the groove overlapping in second layer structure and third layer structure；

   The five-layer structure forms mixing chamber.
8. 8. synthesis system according to claim 7, which is characterized in that

   Have on the bottom surface of first layer structure cavity (L12), the aperture (L11) in the cavity (L12), the cavity (L12) with The diversion cavity (L21) is corresponding.
9. 9. synthesis system according to claim 5, which is characterized in that

   Heat exchange fluid jacket is enclosed with outside the channel of the microreactor, the microreactor includes the bringing-up section being linked in sequence And condensation segment, heating fluid are flowed through out of bringing-up section casing, cooling fluid is flowed through out of condensation segment casing；

   Inserted with ultrasonic transmitter in the casing of the microreactor.
10. 10. synthesis system according to claim 5, which is characterized in that further include:

    Collection vessel (10) is connected to after reaction unit (7)；

    For the counterbalance valve (9) of boosting, the counterbalance valve (9) is mounted at the top of collection vessel (10).