Reaction tube, forming method, reactor and application

Abstract

The invention relates to a reaction tube, a forming method, a reactor and application. The reaction tube comprises a cavity structure enclosed by a continuous surface formed by the edge of the inlet surface, the edge of the compression surface and the edge of the outlet surface; a right-hand three-dimensional rectangular coordinate system is established with the main flowing direction of fluid as the positive direction of the X axis, the compression face is parallel to the Y axis, and the compression face and the positive direction of the X axis form an included angle theta which is larger than or equal to 10 degrees and smaller than or equal to 170 degrees. The vertical section A'of the compression surface A and the vertical section B 'of the compression surface B form a dihedral angle phi, phi is not equal to 0, the longest line segment a on the compression surface A is on the vertical section A', and the longest line segment b on the compression surface B is on the vertical section B '. According to the scaling reaction tube disclosed by the invention, a straight flat tube section of a traditional crossed flat tube is eliminated, and more compression sections can be arranged on pipelines with the same length. According to the reactor, mixing of fluid in the pipe is remarkably enhanced, so that the reaction is more uniform, and heat transfer is more efficient.

Description

Technical Field

[0001] The invention relates to a reaction tube, a molding method, a reactor and applications. Background Art

[0002] There are some process in chemical industry production that have high requirements for fluid mixing and heat transfer. A typical example is rapid chemical reaction. To achieve stable and controllable reaction and ideal reaction selectivity, continuous and uniform mixing and efficient heat transfer are often required. In order to achieve these goals, people have developed various tubular reactors, among which the typical one is the continuous flow reactor. The characteristic dimension of its reaction channel is generally millimeter, so it has a very high specific surface area. At the same time, its reaction channel often has a mixing function. Even at a lower flow rate, it can achieve continuous mixing of fluids and forced convection heat transfer, so it can achieve a narrow residence time distribution of reactants and stable and controllable reaction temperature. Due to these obvious advantages, continuous flow reactors are increasingly widely used.

[0003] Continuous flow reactors can be made of different materials, such as metal (mainly various corrosion-resistant stainless steels and alloys), glass, and silicon carbide. These materials have good heat transfer properties, which is conducive to the transfer of reaction heat. Compared with the latter two materials, metal has better processing toughness and pressure resistance, the reactor is easier to manufacture and safer to use, and the reactor can be repeatedly disassembled and cleaned, easy to maintain, and more reliable and efficient for long-term use.

[0004] At present, continuous flow reactors made of metal materials can be divided into two types. One is to use round tubes or rectangular flat tubes as reaction channels with mixing components added inside; the other is to use various enhanced heat transfer tubes (such as transverse groove tubes, spiral groove tubes, spiral flat tubes, zoom tubes, etc.) as reaction channels. Compared with the latter, due to the presence of internal mixing components, the former has a better forced mixing effect, especially at lower flow rates, which can make the reactants form a narrow residence time distribution; at the same time, the mixing components occupy part of the volume inside the tube, which correspondingly increases the specific surface area per unit reaction volume. Therefore, to achieve the same heat exchange efficiency, the former can use a larger tube diameter. Compared with the former, the main advantage of the latter is that there is no complex internal mixing component, and because the tube itself has a thermal compensation mechanism, a single reaction pipeline can be longer, so the manufacturing process of the reactor is simpler and the cost is lower.

[0005] A cross-flat tube is a type of convergent tube, which is composed of multiple elliptical cross-section tube sections with intersecting axes and some smooth circular cross-section tube sections, with transition sections between adjacent tube sections. When the flow passes through the transition section of the cross-flat tube, the flow cross-section gradually expands in one direction and gradually shrinks in the other direction, and the flow direction and flow velocity of each fluid unit are forced to change, thereby achieving the purpose of forced convection. Chinese patent CN1447088A recommends that the ratio of the long and short axis diameters of the cross-flat tube elliptical cross-section tube section be 1.3-1.7, and the ratio of the length of each elliptical cross-section tube section to the inner diameter of the base tube be 2-3. In order to enhance heat transfer, Chinese patent CN1447089A further proposes that the ratio of the length of the elliptical cross-section tube section to the inner diameter of its base tube should be controlled to 0.05-1. The elliptical flat tube section of the cross flat tube mainly plays the role of heat transfer. When used as a continuous flow reaction channel, it brings several disadvantages: first, the flow velocity and flow direction of the fluid are distributed axially; second, the compression ratio of the original tube cannot be too high. These disadvantages inhibit the mixing of the fluid in the pipeline and thus weaken the heat transfer. Summary of the invention

[0006] The technical problem to be solved by the present invention is to overcome the technical defect that the existing cross flat tubes are not conducive to fluid mixing and heat transfer, and to provide a reaction tube, a molding method, a reactor and applications.

[0007] The present invention solves the above technical problems through the following technical solutions:

[0008] In a first aspect, the present invention provides a reaction tube, which includes a cavity structure surrounded by a continuous surface formed by an edge of an inlet surface, an edge of a compression surface, and an edge of an outlet surface;

[0009] Taking the main flow direction of the fluid as the positive direction of the X-axis, a right-handed three-dimensional rectangular coordinate system is established, the compression surface is parallel to the Y-axis, and the compression surface forms an angle θ with the positive direction of the X-axis, 10°≤θ≤170°;

[0010] The number of the compression surfaces is at least one; when the number of the compression surfaces is at least two, there are adjacent compression surfaces A and B on the reaction tube that satisfy the following relationship: the vertical section A' of the compression surface A and the vertical section B' of the compression surface B form a dihedral angle φ, φ≠0, the longest line segment a on the compression surface A is on the vertical section A', and the longest line segment b on the compression surface B is on the vertical section B'.

[0011] [Shapes of inlet, outlet and compression surfaces]

[0012] In the present invention, the longest line segment L on the compression surface and the line segment h on the compression surface that is perpendicular to the longest line segment L may satisfy a length relationship of L / h=(1.5-10):1.

[0013] In the present invention, when the number of the compression surfaces is at least two, the shape of the cross section of the cavity structure formed by the continuous surface formed by the edges of any two compression surfaces on the reaction tube perpendicular to the X-axis may be different from the shape of the cross section formed by the inlet surface perpendicular to the X-axis.

[0014] In the present invention, when the number of the compression surfaces is at least two, the shape of the cross section of the cavity structure formed by the continuous surface formed by the edges of any two compression surfaces on the reaction tube perpendicular to the X-axis may be different from the shape of the cross section formed by the outlet surface perpendicular to the X-axis.

[0015] In some specific embodiments of the present invention, the inlet surface is circular in shape.

[0016] In some specific embodiments of the present invention, the shape of the outlet surface is circular.

[0017] In some specific embodiments of the present invention, the shape of the compression surface is elliptical or approximately elliptical.

[0018] In the present invention, preferably, L / h=(1.5-5):1, such as 1.9:1, 2.8:1 or 4.4:1.

[0019]

Compression surface angle

[0020] In the present invention, θ may be ≠90°, preferably, 10°≤θ≤80° or 100°≤θ≤170°. According to the conventional definition of angle, θ specifically refers to the angle formed by rotating the positive direction of the X-axis counterclockwise along the XZ plane and the first arrived compression surface.

[0021] In the present invention, preferably, 60°≤θ≤120°, more preferably, 60°≤θ≤90°, for example, θ=60°, 75° or 90°.

[0022] In the present invention, when the number of the compression surfaces is at least two, any adjacent compression surfaces A and B on the reaction tube may satisfy the following relationship: the vertical section A' of the compression surface A and the vertical section B' of the compression surface B form a dihedral angle φ, φ≠0.

[0023] In the present invention, preferably, 10°≤φ≤170°, more preferably 10°≤φ≤90°, for example, φ=60° or 90°. According to the conventional definition of angle, φ specifically refers to the angle formed by the original vertical section A' of the compression surface A and the vertical section B' reached for the first time when the section A is rotated counterclockwise around the X-axis.

[0024] In a specific embodiment of the present invention, when the number of the compression surfaces is at least two, the angles θ formed by each compression surface and the positive direction of the X-axis are the same.

[0025] In a specific embodiment of the present invention, when the number of the compression surfaces is at least three, the dihedral angles φ formed by the perpendicular cross sections of adjacent compression surfaces are all the same.

[0026]

size

[0027] In the present invention, the ratio of the length of the reaction tube to the inner diameter of the reaction tube may be (100-5000):(5-100), for example, 200:5 or 500:11.

[0028] In the present invention, when the number of the compression surfaces is at least two, the ratio of the inner diameter of the reaction tube to the spacing between the centers of adjacent compression surfaces along the reaction tube may be 1:(0.5-10). [Preferred Embodiment]

[0029] In a specific embodiment of the present invention, the number of the compression surfaces is at least two; L:h=1.9:1, θ=90°, φ=90°.

[0030] In a specific embodiment of the present invention, the number of the compression surfaces is at least two; L:h=2.1:1, θ=60°, φ=90°.

[0031] In a specific embodiment of the present invention, the number of the compression surfaces is at least two; L:h=2.8:1, θ=75°, φ=90°.

[0032] In a specific embodiment of the present invention, the number of compression surfaces is at least five; in the first compression surface: L:h=4.4:1, θ=90°, in the second compression surface: L:h=2.8:1, θ=75°, in the third compression surface: L:h=2.1:1, θ=60°, in the fourth compression surface: L:h=2.8:1, θ=75°, in the fifth compression surface: L:h=4.4:1, θ=90°; between the first compression surface and the second compression surface: φ=90°, between the second compression surface and the third compression surface: φ=60°, between the third compression surface and the fourth compression surface: φ=90°, between the fourth compression surface and the fifth compression surface: φ=60°.

[0033] In a second aspect, the present invention provides a method for forming a reaction tube as described above, comprising the following steps: pressing a pipe with a strip clamp, wherein the strip clamp forms an angle θ1 with the positive direction of the X-axis, 10°≤θ1≤170°;

[0034] When the number of the compression surfaces is at least two, the forming method of the reaction tube further includes the following steps: rotating the tube axially by an angle φ, and then pressing the tube with a strip clamp, wherein the strip clamp forms an angle θ2 with the positive direction of the X-axis, 10°≤θ2≤170°.

[0035] In the present invention, the pipe is a round tube and the compression surface is an ellipse. The reaction tube is formed by pressing a round tube at a certain interval, the ratio of the major axis to the minor axis of each compression surface can be the same or different, the angle θ of the inclination angle formed by the major axis of each compression surface and the X-axis can be the same or different, and the intersection angle φ of adjacent compression surfaces can be the same or different.

[0036] In a third aspect, the present invention provides a reactor comprising at least one reaction tube as described above.

[0037] In the present invention, when the number of the reaction tubes is at least two, the reaction tubes may be connected in series or in parallel.

[0038] In the present invention, conventionally, the reactor may further include a shell.

[0039] In a fourth aspect, the present invention provides a use of the reactor as described above in a continuous flow reaction.

[0040] In the present invention, when the fluid enters the inlet surface of the first reaction tube, the Reynolds number Re can be less than 2300.

[0041] The positive and progressive effects of the present invention are:

[0042] (1) The zoomable reaction tube of the present invention eliminates the straight flat tube section of the traditional cross flat tube, and more compression surfaces can be set on the pipeline of the same length;

[0043] (2) The zoomable reaction tube of the present invention has no straight flat tube section, so the time for the fluid to flow through the compression surface is very short, the fluid resistance is reduced, and the compression surface can be set with a larger ratio of long and short axes;

[0044] (3) In the zoom-in reaction tube of the present invention, the long axis of the compression surface intersects with the axis of the base tube to form a certain angle. On the one hand, the flow cross-sectional area of ​​the compression surface is increased, reducing the pressure drop of the fluid passing through the compression surface. On the other hand, the flow direction and flow velocity of the fluid are no longer symmetrically distributed along the tube axis, thereby enhancing the disturbance and mixing of the fluid.

[0045] (4) In the zoom reaction tube of the present invention, the transition section between adjacent compression surfaces is a continuous and smooth transition without a dead zone;

[0046] (5) The reactor of the present invention significantly enhances the mixing of the fluid in the tube, making the reaction more uniform and the heat transfer more efficient. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] Figure 1 This is a front view of the reaction tube of Example 1;

[0048] Figure 2 is a cross-sectional view of the compression surface A on the reaction tube of Example 1;

[0049] Figure 3 is a side cross-sectional view of the reaction tube of Example 1;

[0050] Figure 4a is a stereoscopic view of the reaction tube of Example 1-1;

[0051] Figure 4b is a side cross-sectional view of the reaction tube of Example 1-1;

[0052] Figure 5a is a stereoscopic view of the reaction tube of Example 1-2;

[0053] Figure 5b is a side cross-sectional view of the reaction tube of Example 1-2;

[0054] Figure 6a is a stereoscopic view of the reaction tube of Example 1-3;

[0055] Figure 6b is a side cross-sectional view of the reaction tube of Example 1-3;

[0056] Figure 7a is a stereoscopic view of the reaction tube of Example 1-4;

[0057] Figure 7b is a side cross-sectional view of the reaction tube of Example 1-4;

[0058] Figure 8a is a stereogram of the reaction tube of Example 1-5;

[0059] Figure 8b is a side cross-sectional view of the reaction tube of Example 1-5;

[0060] Fig. 9 is a schematic diagram of the series reactor of Example 2;

[0061] Fig.10 is a schematic diagram of the parallel reactors of Example 2;

[0062] Fig.11 is a schematic diagram of the reactor of Example 2-1;

[0063] The numbers in the figure are as follows: inlet 1, transition section 2, outlet 3, reaction tube 4, and shell 5. DETAILED DESCRIPTION

[0064] A preferred embodiment is given below, and the present invention is described more clearly and completely in conjunction with the accompanying drawings.

[0065] Example 1

[0066] A continuously variable cross-sectional zoom reaction tube, such as Figure 1-3, including a cavity structure surrounded by a continuous surface formed by the edge of the inlet surface, the edge of the compression surface and the edge of the outlet surface; the cross section formed by the inlet 1 of the reaction tube perpendicular to the X-axis is the inlet surface. A transition section 2 is formed between the adjacent compression surfaces A and B. The cross section formed by the outlet 3 of the reaction tube perpendicular to the X-axis is the outlet surface. The shape of the inlet surface is circular. The shape of the outlet surface is circular. The shape of the compression surface is approximately elliptical, and the longest line segment L on the compression surface and the line segment h on the compression surface perpendicular to the longest line segment L satisfy a length relationship of 2.1:1, 3:1 or 4.8:1.

[0067] With the main flow direction of the fluid as the positive direction of the X-axis, a right-handed three-dimensional rectangular coordinate system is established, the compression surface is parallel to the Y-axis, and the number of compression surfaces is about ten; the compression surface forms an angle θ with the positive direction of the X-axis, θ = about 60°;

[0068] On the reaction tube, any two adjacent compression surfaces satisfy the following relationship: the shape of the cross section of the cavity structure formed by the continuous surface formed by the edges of the two compression surfaces perpendicular to the X-axis is different from the shape of the cross section formed by the inlet surface or the outlet surface perpendicular to the X-axis;

[0069] Any adjacent compression surface A and compression surface B satisfy the following relationship: the vertical section A' of the compression surface A and the vertical section B' of the compression surface B form a dihedral angle φ, φ=about 90°, the longest line segment a on the compression surface A is on the vertical section A', and the longest line segment b on the compression surface B is on the vertical section B'.

[0070] Example 1-1: θ is 90°, φ is 90°

[0071] A continuously variable cross-sectional zoom reaction tube, reference Figure 4a and Figure 4b , a circular tube is pressed at a specific position to form a cavity structure surrounded by a continuous surface formed by the edge of the inlet surface, the edge of the compression surface and the edge of the outlet surface;

[0072] The edges of the inlet and outlet surfaces are circular ring structures with an outer diameter of 6 mm, 10 mm or 12 mm and an inner diameter of 5 mm, 9 mm or 11 mm. The length of the reaction tube is 200 mm or 500 mm. There are multiple compression surfaces, which are elliptical, and the length ratio of the major axis to the minor axis of the ellipse, i.e., the compression ratio L / h=1.9:1. The spacing between the center points of adjacent compression surfaces along the reaction tube is 20 mm.

[0073] A right-handed three-dimensional rectangular coordinate system is established with the main flow direction of the fluid as the positive direction of the X-axis; the compression surface is parallel to the Y-axis, and the compression surface forms an angle θ with the X-axis, θ=90°.

[0074] The adjacent compression surfaces A1 and B1 satisfy the following relationship:

[0075] The vertical section A1' of the compression surface A1 and the vertical section B1' of the compression surface B1 form a dihedral angle φ, φ=90°, the major axis a1 of the ellipse on the compression surface A1 is on the vertical section A1', and the major axis b1 of the ellipse on the compression surface B1 is on the vertical section B1'.

[0076] Example 1-2: θ is 60°, φ is 90°

[0077] A continuously variable cross-sectional zoom reaction tube, reference Figure 5a and Figure 5b , a circular tube is pressed at a specific position to form a cavity structure surrounded by a continuous surface formed by the edge of the inlet surface, the edge of the compression surface and the edge of the outlet surface;

[0078] The edges of the inlet and outlet surfaces are circular ring structures with an outer diameter of 6 mm, 10 mm or 12 mm and an inner diameter of 5 mm, 9 mm or 11 mm. The length of the reaction tube is 200 mm or 500 mm. There are multiple compression surfaces, which are elliptical, and the length ratio of the major axis to the minor axis of the ellipse, i.e., the compression ratio L / h=2.1:1. The spacing between the center points of adjacent compression surfaces along the reaction tube is 20 mm.

[0079] A right-handed three-dimensional rectangular coordinate system is established with the main flow direction of the fluid as the positive direction of the X-axis; the compression surface is parallel to the Y-axis, and the compression surface forms an angle θ with the positive direction of the X-axis, θ=60°.

[0080] The adjacent compression surfaces A2 and B2 satisfy the following relationship:

[0081] The vertical section A2' of the compression surface A2 and the vertical section B2' of the compression surface B2 form a dihedral angle φ, φ=90°, the major axis a2 of the ellipse on the compression surface A2 is on the vertical section A2', and the major axis b2 of the ellipse on the compression surface B2 is on the vertical section B2'.

[0082] Example 1-3: θ is 75°, φ is 90°

[0083] A continuously variable cross-sectional zoom reaction tube, reference Figure 6a and Figure 6b , a circular tube is pressed at a specific position to form a cavity structure surrounded by a continuous surface formed by the edge of the inlet surface, the edge of the compression surface and the edge of the outlet surface;

[0084] The edges of the inlet and outlet surfaces are circular ring structures with an outer diameter of 6 mm, 10 mm or 12 mm and an inner diameter of 5 mm, 9 mm or 11 mm. The length of the reaction tube is 200 mm or 500 mm. There are multiple compression surfaces, which are elliptical, and the length ratio of the major axis to the minor axis of the ellipse, i.e., the compression ratio L / h=2.8:1. The spacing between the center points of adjacent compression surfaces along the reaction tube is 12.5 mm.

[0085] A right-handed three-dimensional rectangular coordinate system is established with the main flow direction of the fluid as the positive direction of the X-axis; the compression surface is parallel to the Y-axis, and the compression surface forms an angle θ with the positive direction of the X-axis, θ=75°.

[0086] The adjacent compression surfaces A3 and B3 satisfy the following relationship:

[0087] The vertical section A3' of the compression surface A3 and the vertical section B3' of the compression surface B3 form a dihedral angle φ, φ=90°, the major axis a3 of the ellipse on the compression surface A3 is on the vertical section A3', and the major axis b3 of the ellipse on the compression surface B3 is on the vertical section B3'.

[0088] Embodiment 1-4: θ is 90°, 75°, 60°, 75°, 90°, and φ is 90°, 60°, 90°, 60°

[0089] A continuously variable cross-sectional zoom reaction tube, reference Figure 7a and Figure 7b , a circular tube is pressed at a specific position to form a cavity structure surrounded by a continuous surface formed by the edge of the inlet surface, the edge of the compression surface and the edge of the outlet surface;

[0090] The edges of the inlet and outlet surfaces are circular ring structures with an outer diameter of 6 mm, 10 mm or 12 mm and an inner diameter of 5 mm, 9 mm or 11 mm. The length of the reaction tube is 200 mm or 500 mm. The number of compression surfaces is multiple, and the compression surfaces are elliptical. The spacing between the center points of adjacent compression surfaces along the reaction tube is 12.5 mm.

[0091] With the main flow direction of the fluid as the positive direction of the X-axis, a right-handed three-dimensional rectangular coordinate system is established; the compression surface is parallel to the Y-axis.

[0092] (1) The adjacent compression surfaces A4 and B4 satisfy the following relationship:

[0093] The compression surface A4 is the first compression surface in the positive direction of the X-axis. The length ratio of the major axis to the minor axis of the ellipse of the compression surface A4, i.e., the compression ratio L / h=4.4:1. The compression surface A4 forms an angle θ with the X-axis, θ=90°. The length ratio of the major axis to the minor axis of the ellipse of the compression surface B4, i.e., the compression ratio L / h=2.8:1. The compression surface B4 forms an angle θ with the positive direction of the X-axis, θ=75°.

[0094] The vertical section A4' of the compression surface A4 and the vertical section B4' of the compression surface B4 form a dihedral angle φ, φ=90°, the major axis a4 of the ellipse on the compression surface A4 is on the vertical section A4', and the major axis b4 of the ellipse on the compression surface B4 is on the vertical section B4'.

[0095] (2) The adjacent compression surfaces B4 and C4 satisfy the following relationship:

[0096] The length ratio of the major axis to the minor axis of the ellipse of the compression surface C4, that is, the compression ratio L / h = 2.1: 1. The compression surface C4 forms an angle θ with the positive direction of the X axis, θ = 60°.

[0097] The vertical section B4' of the compression surface B4 and the vertical section C4' of the compression surface C4 form a dihedral angle φ along the positive direction of the Y axis and the positive direction of the Z axis, φ=60°, and the major axis c4 of the ellipse on the compression surface C4 is on the vertical section C4'.

[0098] ③ The adjacent compression surfaces C4 and D4 satisfy the following relationship:

[0099] The length ratio of the major axis to the minor axis of the ellipse of the compression surface D4, that is, the compression ratio L / h = 2.8: 1. The compression surface D4 forms an angle θ with the positive direction of the X axis, θ = 75°.

[0100] The vertical cross section C4' of the compression surface C4 and the vertical cross section D4' of the compression surface D4 form a dihedral angle φ, φ=90°, and the major axis d4 of the ellipse on the compression surface D4 is on the vertical cross section D4'.

[0101] ④ The adjacent compression surfaces D4 and E4 satisfy the following relationship:

[0102] The length ratio of the major axis to the minor axis of the ellipse of the compression surface E4, that is, the compression ratio L / h = 4.4: 1. The compression surface E4 forms an angle θ with the X axis, θ = 90°.

[0103] The vertical section D4' of the compression surface D4 and the vertical section E4' of the compression surface E4 form a dihedral angle φ along the positive direction of the Y axis and the positive direction of the Z axis, φ=60°, and the major axis e4 of the ellipse on the compression surface E4 is on the vertical section E4'.

[0104] Embodiment 1-5: θ is 75°, φ is 60°

[0105] A continuously variable cross-sectional zoom reaction tube, reference Figure 8a and Figure 8b , a circular tube is pressed at a specific position to form a cavity structure surrounded by a continuous surface formed by the edge of the inlet surface, the edge of the compression surface and the edge of the outlet surface;

[0106] The edges of the inlet and outlet surfaces are circular ring structures with an outer diameter of 6 mm, 10 mm or 12 mm and an inner diameter of 5 mm, 9 mm or 11 mm. The length of the reaction tube is 200 mm or 500 mm. There are multiple compression surfaces, which are elliptical, and the length ratio of the major axis to the minor axis of the ellipse, i.e., the compression ratio L / h=2.8:1. The spacing between the center points of adjacent compression surfaces along the reaction tube is 12.5 mm.

[0107] A right-handed three-dimensional rectangular coordinate system is established with the main flow direction of the fluid as the positive direction of the X-axis; the compression surface is parallel to the Y-axis, and the compression surface forms an angle θ with the positive direction of the X-axis, θ=75°.

[0108] The adjacent compression surfaces A5 and B5 satisfy the following relationship:

[0109] The vertical section A5' of the compression surface A5 and the vertical section B5' of the compression surface B5 form a dihedral angle φ, φ=60°, the major axis a5 of the ellipse on the compression surface A5 is on the vertical section A5', and the major axis b5 of the ellipse on the compression surface B5 is on the vertical section B5'.

[0110] Example 2

[0111] A continuous flow reactor comprises a housing 5 and four series-connected Fig. 9 , or four in parallel, such as Fig.10 The reaction tube of Example 1-1, Example 1-2, Example 1-3, Example 1-4 or Example 1-5.

[0112] Example 2-1

[0113] A continuous flow reactor, such as Fig.11 , comprising a shell 5 and a reaction tube of Example 1-1, Example 1-2, Example 1-3 or Example 1-4, the reaction tube has a length of 200 mm, an outer diameter of 6 mm, and an inner diameter of 5 mm.

[0114] Example 2-2

[0115] A continuous flow reactor comprises six reaction tubes of Example 1-1, Example 1-2, Example 1-3 or Example 1-4 connected in series, wherein the reaction tubes have a length of 500 mm, an outer diameter of 12 mm, and an inner diameter of 11 mm.

[0116] Application example: Synthesis of 5-pyrimidineboronic acid

[0117] A 5-bromopyrimidine-tetrahydrofuran solution with a flow rate of 20 mL / min and a molar concentration of 0.5 mol / L and a butyl lithium-n-hexane solution with a flow rate of 4.1 mL / min and a molar concentration of 2.93 mol / L were precooled to -65°C through two heat exchangers, respectively, and injected into the first continuous flow reactor for mixing. Subsequently, the solution was mixed and reacted with a boric acid n-butyl ester-tetrahydrofuran solution with a flow rate of 20 mL / min and a molar concentration of 0.6 mol / L precooled to -55°C through another heat exchanger through the second continuous flow reactor, and the reaction temperature of the two continuous flow reactors was controlled at -50°C.

[0118] Working condition 1: The first continuous flow reactor uses one reaction tube of Example 1-1, the length of the reaction tube is 200 mm, the outer diameter of the round tube is 6 mm, and the inner diameter is 5 mm. The second continuous flow reactor uses six reaction tubes of Example 1-1 in parallel, the length of the reaction tube is 500 mm, the outer diameter is 12 mm, the inner diameter is 11 mm, and the reaction yield is 71%.

[0119] Working condition 2: The first continuous flow reactor uses one reaction tube of Example 1-2, the length of the reaction tube is 200 mm, the outer diameter of the round tube is 6 mm, and the inner diameter is 5 mm. The second continuous flow reactor uses six reaction tubes of Example 1-2 in series, the length of the reaction tube is 500 mm, the outer diameter is 12 mm, the inner diameter is 11 mm, and the reaction yield is 76%.

[0120] Working condition 3: The first continuous flow reactor uses one reaction tube of Example 1-3, the length of the reaction tube is 200 mm, the outer diameter of the round tube is 6 mm, and the inner diameter is 5 mm. The second continuous flow reactor uses six reaction tubes of Example 1-3 in series, the length of the reaction tube is 500 mm, the outer diameter is 12 mm, the inner diameter is 11 mm, and the reaction yield is 89%.

[0121] Working condition 4: The first continuous flow reactor uses one reaction tube of Example 1-4, the length of the reaction tube is 200 mm, the outer diameter of the round tube is 6 mm, and the inner diameter is 5 mm. The second continuous flow reactor uses six reaction tubes of Example 1-4 in series, the length of the reaction tube is 500 mm, the outer diameter is 12 mm, the inner diameter is 11 mm, and the reaction yield is 87%.

[0122] Working condition 5: The first continuous flow reactor uses a reaction tube of Example 1-5, the length of the reaction tube is 200 mm, the outer diameter of the round tube is 6 mm, and the inner diameter is 5 mm. The second continuous flow reactor uses six reaction tubes of Example 1-5 connected in series, the length of the reaction tube is 500 mm, the outer diameter is 12 mm, the inner diameter is 11 mm, and the reaction yield is 82%.

[0123] Among them, the yield of 5-pyrimidineboric acid = molar flow rate of 5-pyrimidineboric acid / molar flow rate of 5-bromopyrimidine. In summary, the reactor formed by the reaction tube of the present invention can form a better flow condition, so that the reaction yield reaches at least 70% or even close to 90%.

Claims

1. A reaction tube, characterized in that: It includes a cavity structure surrounded by a continuous surface formed by the edge of the inlet surface, the edge of the compression surface and the edge of the outlet surface; Taking the main flow direction of the fluid as the positive direction of the X-axis, a right-handed three-dimensional rectangular coordinate system is established, the compression surface is parallel to the Y-axis, and the compression surface forms an angle θ with the positive direction of the X-axis, 10°≤θ≤170°; The number of the compression surfaces is at least one; when the number of the compression surfaces is at least two, there are adjacent compression surfaces A and B on the reaction tube that satisfy the following relationship: the vertical section A' of the compression surface A and the vertical section B' of the compression surface B form a dihedral angle φ, φ≠0, the longest line segment a on the compression surface A is on the vertical section A', and the longest line segment b on the compression surface B is on the vertical section B'.

2. The reaction tube according to claim 1, characterized in that: The longest line segment L on the compression surface and the line segment h on the compression surface that is perpendicular to the longest line segment L satisfy the length relationship L / h=(1.5-10):

1.

3. The reaction tube according to claim 1, characterized in that: When the number of the compression surfaces is at least two, the shape of the cross section of the cavity structure formed by the continuous surface formed by the edges of any two compression surfaces on the reaction tube perpendicular to the X-axis may be different from the shape of the cross section formed by the inlet surface perpendicular to the X-axis; When the number of the compression surfaces is at least two, the shape of the cross section of the cavity structure formed by the continuous surface formed by the edges of any two compression surfaces on the reaction tube perpendicular to the X-axis may be different from the shape of the cross section formed by the outlet surface perpendicular to the X-axis.

4. The reaction tube according to claim 1, characterized in that: When the number of the compression surfaces is at least two, the angles θ formed by each compression surface and the positive direction of the X-axis are the same.

5. The reaction tube according to claim 1, characterized in that: When the number of the compression surfaces is at least three, the dihedral angles φ formed by the perpendicular cross sections of adjacent compression surfaces are all the same.

6. The reaction tube according to claim 1, characterized in that: The shape of the compression surface is elliptical or approximately elliptical.

7. The reaction tube according to claim 1, characterized in that: It satisfies one of the following conditions: ① θ≠90°, preferably, 10°≤θ≤80° or 100°≤θ≤170°; ②60°≤θ≤120°, preferably, 60°≤θ≤90°, for example, θ=60°, 75° or 90°.

8. The reaction tube according to claim 1, characterized in that: 10°≤φ≤170°, more preferably 10°≤φ≤90°, for example, φ=60° or 90°.

9. The reaction tube according to claim 1, characterized in that: When the number of the compression surfaces is at least two, the ratio of the inner diameter of the reaction tube to the spacing between the centers of adjacent compression surfaces along the reaction tube is 1:(0.5-10).

10. A method for forming a reaction tube according to any one of claims 1 to 9, characterized in that: It includes the following steps: Pressing on a pipe with a strip clamp, the strip clamp forms an angle θ1 with the positive direction of the X-axis, 10°≤θ1≤170°; When the number of the compression surfaces is at least two, the forming method of the reaction tube further includes the following steps: rotating the tube axially by an angle φ, and then pressing the tube with a strip clamp, wherein the strip clamp forms an angle θ2 with the positive direction of the X-axis, 10°≤θ2≤170°.

11. A reactor, characterized in that: It comprises at least one reaction tube according to any one of claims 1 to 9.

12. The reactor according to claim 11, characterized in that When the number of the reaction tubes is at least two, the reaction tubes may be connected in series or in parallel; The reactor also includes a housing.

13. Use of the reactor according to claim 11, characterized in that: It is used in continuous flow reactions.

14. Use of the reactor according to claim 13, characterized in that When the fluid enters the inlet surface of the first reaction tube, the Reynolds number Re<2300.

Images