Continuous reactor suitable for high viscosity and high solid content reaction system and its application

Abstract

The present invention relates to a continuous reactor suitable for a high-viscosity and high-solid content reactant system and its application. The continuous reactor comprises a shell, a flow guide cone, an inner sleeve, a structured packing, a gas distributor, and a hydrocyclone; a gas distributor is arranged at the bottom of the reactor, a flow guide cone and an inner sleeve are arranged in the middle, and a hydrocyclone and other reaction internals are arranged at the top of the reactor; the flow guide cone is divided into a contraction type flow guide cone and a divergence type flow guide cone, the contraction type flow guide cone makes the fluid contract inward, and the divergence type flow guide cone makes the fluid diverge outward; structured packing is arranged inside part of the inner sleeve and in the area surrounded by part of the inner sleeve and the shell; N M-level reaction stages are horizontally arranged in parallel in the reactor to obtain an M-level N-row reactor, M≤50, N≤50; the present invention utilizes a multi-stage strong circulation field to better achieve the mixing of solid and liquid materials, strengthen the reaction process, and thus improve the reaction conversion rate and reaction rate.

Description

Technical Field

[0001] The invention belongs to the field of chemical engineering reaction engineering, and in particular relates to a continuous reactor suitable for a high-viscosity and high-solid content reaction system and an application thereof. Background Art

[0002] In chemical reactions, the reaction process in which two different phases, liquid and solid, exist at the same time is called liquid-solid reaction. When the viscosity of the reactants or products is greater than 100cp and the solid content is greater than 5%, the increase in viscosity and the increase in solid particles hinder the probability of contact between the reactants, reduce the diffusion, heat transfer and mass transfer between the reactants, and thus require more time and energy consumption to obtain a higher reaction conversion rate. This type of reaction is common in petrochemical, coal chemical, pharmaceutical, pesticide, synthetic resin and other fields.

[0003] In industry, most reaction processes of high-viscosity and high-solid content systems use intermittent mechanical stirring kettles, such as the reactors used in the production of methyl isocyanate, aromatic polyamide, and PTT fiber. The intermittent stirring kettle also has shortcomings and difficulties that are difficult to overcome, such as the stirring effect caused by large-scale expansion and reaction heat transfer. Especially when the viscosity of the material is high, there are more stringent requirements on the type of stirring paddle.

[0004] Screw extruder is another choice for high-viscosity and high-solid content reactants, especially twin-screw reactors, which can handle materials with higher viscosity and have high heat transfer efficiency and surface self-cleaning functions. However, it is not suitable for reaction residence time exceeding 0.5 hours, that is, high-viscosity and high-solid content reactants with long reaction time still need to explore other types of reactors.

[0005] Patent CN102416307B discloses an internal circulation slurry bed reactor, in which 1 to 160 internal cylinders are arranged in the reactor cylinder, and a gas distributor is arranged at the bottom of each internal cylinder. The reaction liquid circulates continuously in the reactor. The reactor increases the number of inner cylinders in the cylinder, which poses certain difficulties when the processing volume is large.

[0006] Patents CN1171667C and CN105400544A both propose a multi-stage loop reactor. The introduction of a multi-stage form is beneficial to the high degree of upward amplification. However, the design of the internal components of the reactor still has a serious defect, that is, since the inner sleeve is always a gas rising zone, the materials in the inner sleeve and the inner wall area of ​​the reactor, especially the solid particulate materials, are prone to short circuit and have no recovery ability. Therefore, the multi-stage loop reactor cannot be used in high-viscosity and high-solid content reactant systems.

[0007] As can be seen from the above, the current industrial reactor for processing high-viscosity and high-solid content reaction systems is still an intermittent stirred tank. The intermittent reaction process requires frequent manual opening of the reactor, resulting in the volatile toxic gases produced by the side reactions in the production process into the atmosphere, affecting the environment and worker safety. The intermittent reaction process parameters are greatly affected by human factors and are difficult to control, resulting in unstable or even unqualified product indicators. The present invention reduces the risk of material leakage and achieves intrinsic safety by inventing a continuous reactor suitable for high-viscosity and high-solid content reaction systems. Summary of the invention

[0008] The purpose of the present invention is to provide a continuous reactor suitable for high-viscosity and high-solid content reaction systems and its application, the reactor can make the gas-liquid-solid three-phase system fully contact, promote mixing, increase the interphase contact area and transfer coefficient, strengthen mass transfer and heat transfer, and improve the conversion rate. The reactor has the characteristics of not easy to block, low energy consumption, large processing capacity per unit cross-sectional area of ​​the reactor, high conversion rate, etc.

[0009] The present invention provides a continuous reactor suitable for high-viscosity and high-solid content reactant systems, the main structure of which is a shell, a guide cone, an inner sleeve, a structured filler, a gas distributor, and a hydrocyclone. The main difference between the reactor and the batch reactor is that by setting reaction internals and introducing inert gas, the reactants are fully contacted under the action of the inert gas and the reaction internals, increasing the interphase contact area and transfer coefficient, strengthening mass transfer and heat transfer, and improving the conversion rate.

[0010] The technical solution of the present invention is as follows:

[0011] A continuous reactor suitable for high-viscosity and high-solid content reactant systems, characterized in that it comprises a shell, a guide cone, an inner sleeve, a structured filler, a gas distributor, and a hydrocyclone separator; a gas distributor is arranged at the bottom of the reactor, a guide cone and an inner sleeve are arranged in the middle, and a hydrocyclone separator and other reaction internals are arranged at the top of the reactor; the guide cone is divided into a contraction guide cone and a divergence guide cone, the contraction guide cone makes the fluid contract inward, and the divergence guide cone makes the fluid diverge outward; structured fillers are arranged inside part of the inner sleeve and in part of the area surrounded by the inner sleeve and the shell; there are two arrangements of the guide cone and the inner sleeve in the reactor, one is the gas distributor, and the other is the gas distributor. The upper part of the distributor is a contraction-type guide cone, the upper part of which is an inner sleeve, and then upwards is a divergence-type guide cone, and then upwards is an inner sleeve, and then upwards is a contraction-type guide cone, and so on, the uppermost part is a hydrocyclone separator; another way is that the upper part of the gas distributor is a divergence-type guide cone, the upper part is an inner sleeve, and then upwards is a contraction-type guide cone, and then upwards is an inner sleeve, and then upwards is a divergence-type guide cone, and so on, the uppermost part is a hydrocyclone separator. Regardless of the arrangement, a structured packing is arranged inside the inner sleeve adjacent to the upper part of the contraction-type guide cone, and a structured packing is arranged in the area surrounded by the inner sleeve adjacent to the upper part of the divergence-type guide cone and the shell.

[0012] The reactor shell is rectangular or circular, and the inner sleeve is circular. When the shell is rectangular, the divergent guide cone and the contraction guide cone are double pyramid structures; when the shell is circular, the divergent guide cone is a double cone structure, and the contraction guide cone is a hollow cylindrical structure.

[0013] The cross-sectional area of ​​the inner sleeve in the reactor accounts for 25% to 75% of the cross-sectional area of ​​the shell; the height of the inner sleeve is 0.5m to 2m, and the gap area between the inner sleeve and the guide cone accounts for 5% to 50% of the area of ​​the inner sleeve; the gap area between the contraction-type guide cones accounts for 10% to 50% of the area of ​​the inner sleeve, and the gap area between the divergence-type guide cone and the shell accounts for 5% to 25% of the area of ​​the inner sleeve.

[0014] The inner sleeve of the reactor and the upper and lower adjacent flow guide cones form a reaction stage, and the reactor includes a primary, secondary or multi-stage reaction stage. The inner sleeve adjacent to the upper part of the contraction-type flow guide cone forms a rising zone of the reaction stage, in which a structured packing is arranged, and the area surrounded by the inner sleeve and the shell forms a descending zone of the reaction stage; the inner sleeve adjacent to the upper part of the divergent flow guide cone and the area surrounded by the shell form a rising zone of the reaction stage, in which a structured packing is arranged, and the inner sleeve forms a descending zone of the reaction stage.

[0015] The reactor is horizontally paralleled with N M-level reaction stages to obtain an M-level N-row reactor, M≤50, N≤50, and the cross-sectional area between the inner sleeves in the horizontal direction is equal to the cross-sectional area of ​​the inner sleeve. The shell of the M-level N-row reactor is rectangular or circular, preferably a rectangular shell when the operating pressure is normal pressure, and preferably a circular shell when the operating pressure is negative pressure or positive pressure; the inner sleeve is a prism, and the guide cones are all divergent guide cones, the guide cones in contact with the shell are prism divergent guide cones, and the guide cones not in contact with the shell are double-pyramid divergent guide cones; when the inner sleeve is a double-pyramid divergent guide cone, the inner sleeve is surrounded by a descending area, and the inner sleeve and the inner sleeve adjacent to the horizontal direction are surrounded by an ascending area, and when the inner sleeve is a gap formed by two adjacent double-pyramid divergent guide cones, the inner sleeve is surrounded by an ascending area, and the inner sleeve and the inner sleeve adjacent to the horizontal direction are surrounded by a descending area; a regular packing for enhanced disturbance is arranged in the ascending area.

[0016] The structured packing is a plate mesh packing with models of 250X, 250Y, 350X, 350Y, 500X, and 500Y.

[0017] The operating temperature of the reactor is room temperature to 450° C., and the operating pressure is an absolute pressure of 10 kPa to 10 MPa.

[0018] The superficial velocity of the gas entering the reactor is 0.01 m / s to 1 m / s.

[0019] The inert gas introduced into the reactor can be any gas that does not chemically react with the reactants, preferably nitrogen.

[0020] The specific instructions are as follows

[0021] A continuous reactor suitable for high-viscosity and high-solid content reactants, including a shell, a guide cone, an inner sleeve, a structured packing, a gas distributor, and a hydrocyclone; a gas distributor is provided at the bottom of the reactor, a guide cone, an inner sleeve, and a structured packing are provided in the middle, and a hydrocyclone and other reaction internals are provided at the top of the reactor; the guide cone is divided into a contraction guide cone and a divergence guide cone, the contraction guide cone makes the fluid contract inward, and the divergence guide cone makes the fluid diverge outward. Structured packing is provided inside part of the inner sleeve and in the area surrounded by part of the inner sleeve and the shell. There are two arrangements of the guide cone and the inner sleeve in the reactor. One is that the upper part of the gas distributor is a contraction-type guide cone, the upper part of which is the inner sleeve, and the upper part is a divergence-type guide cone, and the upper part is the inner sleeve, and the upper part is a contraction-type guide cone, and the upper part is the contraction-type guide cone, and the upper part is the divergence-type guide cone, and the upper part is the contraction-type guide cone, and the upper part is the inner sleeve, and the upper part is the divergence-type guide cone, and the upper part is the hydrocyclone. Regardless of the arrangement, a structured packing is arranged inside the inner sleeve adjacent to the upper part of the contraction-type guide cone, and a structured packing is arranged in the area surrounded by the inner sleeve adjacent to the upper part of the divergence-type guide cone and the shell.

[0022] The inner sleeve, structured packing and the upper and lower adjacent guide cones form a reaction stage. According to the number of inner sleeves arranged in the vertical direction, the reactor is divided into a primary reactor, a secondary reactor or a multi-stage reactor. The structure of the simplest primary reactor is arranged from bottom to top according to the first arrangement mode, which is a gas distributor, a contraction guide cone, an inner sleeve and a regular packing, a divergence guide cone and a hydrocyclone separator; according to the second arrangement mode, from bottom to top, it is a gas distributor, a divergence guide cone, an inner sleeve and a regular packing, a contraction guide cone and a hydrocyclone separator. The inner sleeve adjacent to the upper part of the contraction guide cone forms the rising zone of the reaction stage, in which a structured packing for strengthening disturbance is arranged, and the area surrounded by the inner sleeve and the shell forms the descending zone of the reaction stage; the inner sleeve adjacent to the upper part of the divergence guide cone and the area surrounded by the shell form the rising zone of the reaction stage, in which a structured packing for strengthening is also arranged, and the inner sleeve forms the descending zone of the reaction stage. The secondary reactor is composed of an inner sleeve, a structured packing and a guide cone added to the primary reactor. The specific arrangement is that an inner sleeve, a structured packing and a contraction guide cone are added to the upper part of the divergent guide cone on the inner sleeve of the primary reactor of the first arrangement, or an inner sleeve, a structured packing and a divergent guide cone are added to the upper part of the contraction guide cone on the inner sleeve of the primary reactor of the second arrangement. The number of inner cylinders in the vertical direction of the reactor is 2, among which the lower inner sleeve and the structured packing and the guide cones adjacent to the upper and lower parts form the first reaction stage, the upper inner sleeve and the structured packing and the guide cones adjacent to the upper and lower parts form the second reaction stage, and the guide cone between the two inner sleeves is the common part of the first reaction stage and the second reaction stage. Similarly, when 3 or more inner sleeves and corresponding guide cones are arranged in the vertical direction, a three-stage or multi-stage reactor is formed.

[0023] N M-level reaction stages are arranged in parallel in the reactor to obtain an M-level N-row reactor, M≤50, N≤50, and the cross-sectional area between the inner sleeves in the horizontal direction is equal to the cross-sectional area of ​​the inner sleeve. The shell of the M-level N-row reactor is rectangular or circular, and a rectangular shell is preferred when the operating pressure is normal pressure, and a circular shell is preferred when the operating pressure is negative pressure or positive pressure; the inner sleeve is a prism, and the guide cones are all divergent guide cones, the guide cones in contact with the shell are prism divergent guide cones, and the guide cones not in contact with the shell are double-pyramid divergent guide cones; when the inner sleeve is a double-pyramid divergent guide cone, the inner sleeve is surrounded by a descending zone, and the inner sleeve and the inner sleeves adjacent to it in the horizontal direction are surrounded by an ascending zone, and when the inner sleeve is a gap formed by two adjacent double-pyramid divergent guide cones, the inner sleeve is surrounded by an ascending zone, and the inner sleeve and the inner sleeves adjacent to it in the horizontal direction are surrounded by a descending zone; a regular packing for enhanced disturbance is arranged in the ascending zone.

[0024] A continuous reactor suitable for high-viscosity and high-solid content reactant systems is provided with a gas inlet, an upper feed port, a lower feed port, an upper discharge port, a lower discharge port, and a gas discharge port, wherein a gas distributor is connected to the gas inlet.

[0025] The reactor shell is rectangular or circular. When the shell is rectangular, the divergent guide cone and the contraction guide cone are double pyramid structures; when the shell is circular, the divergent guide cone is a double cone structure, and the contraction guide cone is a hollow cylindrical structure.

[0026] Taking the first arrangement of a primary reactor as an example, when the reaction materials enter from the bottom and exit from the top, the flow pattern of the liquid and solid in the reactor is as follows: one or more reaction materials enter the bottom of the reactor from the lower feed port of the reactor, and the gas enters the reactor from the gas inlet at the bottom of the reactor. After being distributed by the gas distributor, it disturbs the reaction liquid at the bottom of the tower, strengthens the mixing between the reaction liquids and moves upward. The gas flow rate at the center of the contraction-type guide cone is much greater than that at the edge of the contraction-type guide cone. Therefore, the liquid-solid reaction liquid is carried upward by the gas at the center of the contraction-type guide cone, and the liquid-solid reaction liquid moves downward at the edge of the contraction-type guide cone, and then is carried upward by the rising gas from the center of the contraction-type guide cone, that is, the liquid-solid reaction liquid completes a circulation flow at the contraction-type guide cone; the liquid-solid reaction liquid from the contraction-type guide cone continues to move upward and enters the rising area in the inner sleeve, and the divergent guide cone at the upper part of the inner sleeve The flow cone prevents the reaction liquid from continuing to move upward. The liquid-solid reaction liquid moves obliquely upward along the lower cone surface of the divergent guide cone to the farthest point of the guide cone. Part of the liquid-solid reaction liquid is entrained into the descending area outside the inner sleeve due to the action of gravity and a small amount of gas. The contraction guide cone prevents this part of the reaction liquid from continuing to descend. The liquid-solid reaction liquid moves obliquely downward along the upper inclined surface of the contraction guide cone and is carried by a large amount of gas from the center of the contraction guide cone and enters the ascending area inside the inner sleeve again, thereby completing a second circulation flow inside and outside the inner sleeve; in the center of the divergent guide cone and the shell, the liquid-solid reaction liquid is carried by the gas into the upper part of the divergent guide cone. At the edge of the divergent guide cone and the shell, due to the small amount of gas, part of the liquid-solid reaction liquid moves downward from the upper part of the divergent guide cone and is carried by the gas to the upper part of the divergent guide cone again. In this way, the liquid-solid reaction liquid completes another circulation flow in the divergent guide cone. The circulating flow strengthens the mixing of gas, liquid and solid phases, increases the contact probability of reactants, and improves the reaction rate. After the reaction is completed, the liquid-solid reaction liquid is discharged from the reactor from the upper discharge port; when the gas passes through the hydrocyclone separator, the entrained liquid and solid are separated and then discharged from the gas outlet at the top of the reactor.

[0027] Taking the first-stage reactor and the first arrangement as an example, when the reaction materials enter from the top and exit from the bottom, the flow pattern of the fluid in the reactor is as follows: one or more reaction materials enter the upper area of ​​the divergent guide cone from the upper feed port of the reactor, and due to the small amount of gas at the edge of the divergent guide cone and the shell, some liquid-solid reaction liquid will move downward from the upper part of the divergent guide cone, and in the center of the divergent guide cone and the shell, the liquid-solid reaction liquid is carried by a large amount of gas into the upper part of the divergent guide cone, so that the liquid-solid reaction liquid completes a circulation flow between the divergent guide cone and the shell. The liquid-solid reaction liquid from between the divergent guide cone and the shell continues to move downward and enters the descending zone outside the inner sleeve. The contraction guide cone prevents this part of the reaction liquid from continuing to descend. The liquid-solid reaction liquid moves downward along the upper inclined surface of the contraction guide cone and is carried by a large amount of gas from the center of the contraction guide cone into the ascending zone inside the inner sleeve. The divergent guide cone on the upper part of the inner sleeve prevents the reaction liquid from continuing to move upward. The liquid-solid reaction liquid moves upward along the lower conical surface of the divergent guide cone to the farthest point of the guide cone. Part of the liquid-solid reaction liquid is entrained into the descending zone outside the inner sleeve under the action of gravity and a small amount of gas, thereby completing the second circulation flow inside and outside the inner sleeve. ; The gas flow rate at the center of the contraction guide cone is much greater than that at the edge of the contraction guide cone. Therefore, the liquid-solid reaction liquid is carried upward by the gas in the center of the contraction guide cone, and the liquid-solid reaction liquid moves downward at the edge of the contraction guide cone, and is carried upward from the center of the contraction guide cone by the rising gas, that is, the liquid-solid reaction liquid completes a circulation flow again at the contraction guide cone; the circulation flow strengthens the mixing of the gas, liquid and solid phases, increases the contact probability of the reactants, and improves the reaction rate. After the reaction is completed, the liquid-solid reaction liquid is discharged from the reactor from the lower discharge port; when the gas passes through the cyclone separator, the entrained liquid and solid are separated and discharged from the gas outlet at the top of the reactor.

[0028] N M-level reaction stages are arranged horizontally in parallel in the reactor to obtain an M-level N-row reactor, M≤50, N≤50, and the cross-sectional area between the inner sleeves in the horizontal direction is equal to the cross-sectional area of ​​the inner sleeve. The shell of the M-level N-row reactor is rectangular or circular, and a rectangular shell is preferred when the operating pressure is normal pressure, and a circular shell is preferred when the operating pressure is negative pressure or positive pressure; the inner sleeve is a prism, and the guide cones are all divergent guide cones. The guide cones in contact with the shell are prism divergent guide cones, and the guide cones not in contact with the shell are double-pyramid divergent guide cones; when the inner sleeve is a double-pyramid divergent guide cone, the inner sleeve is surrounded by a descending zone, and the inner sleeve and the inner sleeves adjacent to it in the horizontal direction are surrounded by an ascending zone, and when the inner sleeve is a gap formed by two adjacent double-pyramid divergent guide cones, the inner sleeve is surrounded by an ascending zone, and the inner sleeve and the inner sleeves adjacent to it in the horizontal direction are surrounded by a descending zone; a regular packing for enhanced disturbance is arranged in the ascending zone.

[0029] The advantages of the present invention are:

[0030] The disturbance of the gas and the density difference inside and outside the inner sleeve make the three-phase system of reaction liquid, gas, liquid and solid fully contact, promote mixing, increase the interphase contact area and transfer coefficient, enhance mass transfer and heat transfer, and achieve a high conversion rate.

[0031] The solid particles are evenly distributed inside the reactor without local accumulation or deposition. The reactor has a large processing capacity per unit cross-sectional area and is easy to scale up industrially.

[0032] The reaction materials circulate in a directional manner in the ascending and descending zones and between the guide cones. The materials on the surface of the reactor and the inner sleeve are constantly renewed, and the temperature distribution is uniform, which is especially suitable for exothermic reactions.

[0033] The present invention utilizes a multi-stage intense circulation field to better achieve the mixing of solid and liquid materials, strengthen the reaction process, and thus improve the reaction conversion rate and reaction rate. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 Schematic diagram of continuous primary reactor for high viscosity and high solid content reaction system

[0035] Figure 2 Schematic diagram of continuous two-stage reactor for high viscosity and high solid content reaction system

[0036] Figure 3 Schematic diagram of contraction guide cone

[0037] Figure 4 Schematic diagram of divergent guide cone

[0038] Figure 5 Continuous 3-stage 3-row reactor structure for high viscosity and high solid content reactants

[0039] Figure 6 Continuous M-stage N-row reactor structure for high viscosity and high solid content reactants

[0040] Among them: 1-shell, 2-contracting guide cone, 3-inner sleeve, 4-divergent guide cone, 5-structured packing, 6-gas distributor, 7-cyclone, 8-gas inlet, 9-lower feed port, 10-lower discharge port, 11-upper feed port, 12-upper discharge port, 13-gas outlet. DETAILED DESCRIPTION

[0041] The present invention is further described in detail below in conjunction with the accompanying drawings:

[0042] Example 1

[0043] Example 1 is the application of a continuous primary reactor of a high-viscosity and high-solid content reactant system in the synthesis of 2-amino-8-naphthol-6-sulfonic acid.

[0044] like Figure 1 , Figure 3 and Figure 4 As shown:

[0045] The reactor comprises a shell 1, a contraction-type flow guide cone 2, an inner sleeve 3, a divergence-type flow guide cone 4, a structured packing 5, a gas distributor 6, and a hydrocyclone 7; the internal parts of the reactor are, from bottom to top, a gas distributor 6, a contraction-type flow guide cone 2, an inner sleeve 3 and a structured packing 5, a divergence-type flow guide cone 4, and a hydrocyclone 6; the reactor is provided with a gas inlet 8, an upper feed port 11, an upper discharge port 12, a lower feed port 11, a lower discharge port 12, and a gas discharge port 13. The lower flow guide cone of the inner sleeve 3 is a contraction-type flow guide cone 2, the inner sleeve 3 is an ascending zone, and the outer sleeve 3 is a descending zone; a structured packing 5 for enhancing disturbance is provided in the ascending zone.

[0046] The cross-sectional area of ​​the inner sleeve 3 in the reactor accounts for 50% of the cross-sectional area of ​​the shell 1, the height of the inner sleeve 3 is 1.5m, the gap area between the inner sleeve 3 and the contraction-type guide cone 2 or the divergence-type guide cone 4 accounts for 20% of the area of ​​the inner sleeve 3, the gap area between the contraction-type guide cone 2 accounts for 25% of the area of ​​the inner sleeve 3, and the gap area between the divergence-type guide cone 4 and the shell 1 accounts for 25% of the area of ​​the inner sleeve. The structured packing 5 adopts 350X plate mesh packing; the reactor shell 1 is circular, and the contraction-type guide cone 2 adopts Figure 3 The hollow cylindrical structure shown in the figure, the divergent guide cone 4 adopts Figure 4 The double cone structure shown.

[0047] The reactor is applied to the synthesis of 2-amino-8-naphthol-6-sulfonic acid and the effect is as follows: 2-naphthylamine-6,8-disulfonic acid solution and potassium hydroxide and sodium hydroxide in a molar ratio of 1:1:1 are heated to 180°C in a raw material premixing tank and stirred until melted; the premixed liquid enters the reactor through the raw material inlet at the lower part of the reactor at a flow rate of 25kg / h; nitrogen at 200°C is inlet into the reactor from the bottom of the reactor, and the apparent flow rate of nitrogen in the reactor is 0.2m / s; the viscosity of the reactant system is 200cp, and the reactor controls the reaction temperature to 200±5°C through a jacket; the reaction pressure is controlled between 0.3±0.05MPa by controlling the regulating valve of the gas phase at the top of the reactor tower; the reaction residence time is 2h, and the reaction liquid after the reaction is completed is added with water from the product outlet at the upper part of the reactor and flows into the product buffer tank, and enters the acid precipitation process after dilution and cooling; the gas phase at the top of the reactor is removed from the gas washing tank to remove the carried ammonia and phenol impurities, and the nitrogen after absorbing the waste gas is discharged at a high point. After acid precipitation and filtration, the product was analyzed by liquid chromatography to find 98.66% of 2-amino-8-naphthol-6-sulfonic acid and 0.06% of 2-naphthylamine-6,8-disulfonic acid. Compared with the batch reactor, the reaction residence time and product temperature are shortened, and it is easy to scale up.

[0048] Example 2

[0049] Example 2 is the application of a continuous secondary reactor for a high-viscosity and high-solid content reactant system in the synthesis of methyl isocyanate.

[0050] like Figure 2 , Figure 3 and Figure 4 As shown:

[0051] The reactor comprises a shell 1, a contraction-type flow guide cone 2, an inner sleeve 3, a divergence-type flow guide cone 4, a structured packing 5, a gas distributor 6, and a hydrocyclone 7; the internal parts of the reactor are, from bottom to top, a gas distributor 6, a contraction-type flow guide cone 2, an inner sleeve 3 and a structured packing 5, a divergence-type flow guide cone 4, and a hydrocyclone 6; the reactor is provided with a gas inlet 8, an upper feed port 11, an upper discharge port 12, a lower feed port 11, a lower discharge port 12, and a gas discharge port 13. The lower flow guide cone of the lower one of the two inner sleeves 3 is a contraction-type flow guide cone 2, the inner sleeve 3 is an ascending zone, and the outer part of the inner sleeve 3 is a descending zone, and the lower flow guide cone of the higher one of the two inner sleeves 3 is a divergence-type flow guide cone 4, the outer part of the inner sleeve 3 is an ascending zone, and the inner sleeve 4 is a descending zone, and structured packing 5 for strengthening disturbance is provided in all ascending zones.

[0052] The cross-sectional area of ​​the inner sleeve 3 in the reactor accounts for 50% of the cross-sectional area of ​​the shell 1, the height of the inner sleeve 3 is 1m, the gap area between the inner sleeve 3 and the contraction-type guide cone 2 or the divergence-type guide cone 4 accounts for 25% of the area of ​​the inner sleeve 3, the gap area between the contraction-type guide cone 2 accounts for 250% of the area of ​​the inner sleeve 3, and the gap area between the divergence-type guide cone 4 and the shell 1 accounts for 20% of the area of ​​the inner sleeve. The structured packing 5 adopts 250X plate mesh packing; the reactor shell 1 is rectangular, and the contraction-type guide cone 2 adopts Figure 3 The double pyramid structure shown in the figure, the divergent guide cone 4 adopts Figure 4 The double pyramid structure shown,

[0053] The effect of this reactor in the synthesis of methyl isocyanate is as follows:

[0054] 180# solvent oil enters the reactor through the lower feed port at a flow rate of 2000g / h, sodium cyanate 267g / h, and dimethyl sulfate 323g / h. The solid content of the reactants is 28%, and the reaction temperature is controlled at 180°C by the jacket; 180°C nitrogen is imported from the bottom of the reactor, and the apparent flow rate of nitrogen in the reactor is 0.43m / s; the reaction residence time is 2 hours, and other materials after the reaction are taken out from the upper material outlet of the reactor. Nitrogen and the generated methyl isocyanate are condensed and separated to obtain 189g / h of methyl isocyanate; the content of methyl isocyanate is 99.5% by chromatography analysis. The use of this reactor makes the synthesis of methyl isocyanate a continuous operation, reduces the risk of highly toxic gas leakage, improves the operating environment, and improves the inherent safety of the process.

[0055] Example 3

[0056] Example 3 is the application of a continuous three-stage three-row reactor with a high-viscosity and high-solid content reactant system in the synthesis of 2,4-dichlorophenoxyacetic acid from sodium 2,4-dichlorophenol and sodium chloroacetate.

[0057] like Figure 6 As shown:

[0058] M-level N-row reactor M≤50, N≤50, the cross-sectional area between the inner sleeves 3 in the horizontal direction is equal to the cross-sectional area of ​​the inner sleeve 3. The shell 1 of the M-level N-row reactor is rectangular or circular, preferably a rectangular shell when the operating pressure is normal pressure, and preferably a circular shell when the operating pressure is negative pressure or positive pressure; the inner sleeve 3 is a prism, and the guide cones are all divergent guide cones 4, the guide cones in contact with the shell are prism divergent guide cones 4, and the guide cones not in contact with the shell are double-pyramid divergent guide cones 4; when the inner sleeve 3 is a double-pyramid divergent guide cone 4, the inner sleeve 3 is surrounded by a descending area, and the inner sleeve 3 and the inner sleeves 3 adjacent to the horizontal direction are surrounded by an ascending area, and when the inner sleeve 3 is a gap formed by two adjacent double-pyramid divergent guide cones 4, the inner sleeve is surrounded by an ascending area, and the inner sleeve 3 and the inner sleeves 3 adjacent to the horizontal direction are surrounded by a descending area; a structured packing 5 for enhanced disturbance is arranged in the ascending area.

[0059] like Figure 3 , Figure 4 , Figure 5 As shown:

[0060] Among the M-level N-row reactors, M and N are selected as three-level three-row reactors; including a shell 1, a contraction-type flow guide cone 2, an inner sleeve 3, a divergent flow guide cone 4, a structured packing 5, a gas distributor 6, and a hydrocyclone 7; the internal parts of the reactor are, from bottom to top, a gas distributor 6, a divergent flow guide cone 4 or its left and right parts, an inner sleeve 3 and a structured packing 5, a divergent flow guide cone 4, and a hydrocyclone 6; the reactor is provided with a gas inlet 8, an upper feed port 11, an upper discharge port 12, a lower feed port 11, a lower discharge port 12, and a gas discharge port 13. The two inner sleeves 3 at the lower left and the divergent flow guide cones 4 above and below are the secondary reactors of Example 2. On the basis of Example 2, an inner sleeve 3, a structured packing 5, and a divergent flow guide cone 4 are added to obtain a three-level reactor. The three-level reactor is arrayed twice in the horizontal direction to obtain a three-level three-row reactor, and the cross-sectional area between the inner sleeves 3 in the horizontal direction is equal to the cross-sectional area of ​​the inner sleeve 3.

[0061] The cross-sectional area of ​​the inner sleeve 3 in the reactor accounts for 50% of the cross-sectional area of ​​the shell 1, the height of the inner sleeve 3 is 2m, the gap area between the inner sleeve 3 and the divergent flow guide cone 4 accounts for 25% of the area of ​​the inner sleeve 3, the gap area between the contraction flow guide cone 2 accounts for 25% of the area of ​​the inner sleeve 3, and the gap area between the divergent flow guide cone 4 and the shell 1 accounts for 15% of the area of ​​the inner sleeve. The structured packing 5 adopts 500X plate mesh packing; the reactor shell 1 is rectangular, and the divergent flow guide cone 4 adopts Figure 4 The double pyramid diverging guide cone and the prism diverging guide cone are shown.

[0062] Industrially, 2,4-dichlorophenol sodium salt and sodium chlorate are used to synthesize 2,4-dichlorophenoxyacetic acid in an intermittent reactor. The solid content of the reactant system is 30%. The discharge port of the intermittent reactor with 5 reactors in series is easily blocked, which affects the production capacity of the device. The three-stage three-row continuous reactor with a high viscosity and high solid content reactant system of the invention has the following effects:

[0063] The molar ratio of 2,4-dichlorophenol sodium salt to sodium chlorate is 1.1:1, and it enters the reactor through the upper feed port of the reactor. The solid content of the reactant is 30%, and the reaction temperature is controlled at 110°C by the jacket; 110°C nitrogen is imported into the reactor from the bottom of the reactor, and the apparent flow rate of nitrogen in the reactor is 0.28m / s; when the reaction residence time is 6, nitrogen is extracted from the upper material outlet of the reactor, and the solid-liquid mixture is extracted from the lower discharge port of the reactor. Analysis shows that the conversion rate of 2,4-dichlorophenol sodium is 91%. The reactor makes the production of 2,4-dichlorophenoxyacetic acid a continuous and stable operation, avoiding unplanned shutdown caused by blockage of the discharge port of the intermittent reactor. In addition, one vertical reactor replaces five series-connected intermittent reactors, greatly reducing the footprint of the device.

[0064] The above embodiments are only preferred examples for introducing the present invention. For those skilled in the art, any obvious changes and improvements made without departing from the spirit of the present invention should be regarded as part of the present invention.

Claims

1. A continuous reactor suitable for high-viscosity and high-solid content reaction systems, characterized in that: It comprises a shell, a guide cone, an inner sleeve, a structured packing, a gas distributor, and a hydrocyclone separator; a gas distributor is arranged at the bottom of the reactor, a guide cone and an inner sleeve are arranged in the middle, and a hydrocyclone separator reaction internal is arranged at the top of the reactor; the guide cone is divided into a contraction guide cone and a divergence guide cone, the contraction guide cone makes the fluid contract inward, and the divergence guide cone makes the fluid diverge outward; A structured packing is arranged inside the inner sleeve adjacent to the upper part of the contraction-type guide cone, and a structured packing is arranged in the inner sleeve adjacent to the upper part of the divergence-type guide cone and the area surrounded by the shell; there are two arrangements of the guide cone and the inner sleeve in the reactor, one is that the upper part of the gas distributor is a contraction-type guide cone, the upper part of which is the inner sleeve, and the upper part is a divergence-type guide cone, and the upper part is the inner sleeve, and the upper part is a contraction-type guide cone, and so on, and the uppermost part is a hydrocyclone; the other way is that the upper part of the gas distributor is a divergence-type guide cone, the upper part is the inner sleeve, and the upper part is a contraction-type guide cone, and the upper part is the inner sleeve, and the upper part is an inner sleeve, and the upper part is a divergence-type guide cone, and so on, and the uppermost part is a hydrocyclone.

2. The reactor as described in claim 1 is characterized in that the reactor shell is rectangular or circular. When the shell is rectangular, the divergent guide cone and the contraction guide cone are double-pyramid structures; when the shell is circular, the divergent guide cone is a double-conical structure, and the contraction guide cone is a hollow cylindrical structure.

3. The reactor according to claim 1, characterized in that The cross-sectional area of ​​the inner sleeve in the reactor accounts for 25% to 75% of the cross-sectional area of ​​the shell; the height of the inner sleeve is 0.5m to 2m, and the gap area between the inner sleeve and the guide cone accounts for 5% to 50% of the area of ​​the inner sleeve; the gap area between the contraction-type guide cones accounts for 10% to 50% of the area of ​​the inner sleeve, and the gap area between the divergence-type guide cone and the shell accounts for 5% to 25% of the area of ​​the inner sleeve.

4. The reactor according to claim 1, characterized in that The inner sleeve of the reactor and the upper and lower adjacent guide cones form a reaction stage, and the reactor includes a primary, secondary or multi-stage reaction stage; the interior of the inner sleeve adjacent to the upper part of the contraction-type guide cone forms a rising zone of the reaction stage, in which a structured filler is arranged, and the area surrounded by the inner sleeve and the shell forms a descending zone of the reaction stage; the inner sleeve adjacent to the upper part of the divergent-type guide cone and the area surrounded by the shell form a rising zone of the reaction stage, in which a structured filler is arranged, and the interior of the inner sleeve forms a descending zone of the reaction stage.

5. The reactor according to claim 1, characterized in that: M stages and N rows of reaction stages are arranged in parallel in the reactor, M≤50, N≤50, and the cross-sectional area between the inner sleeves in the horizontal direction is equal to the cross-sectional area of ​​the inner sleeve.

6. The reactor according to claim 5, characterized in that: The shell of the M-stage N-row reactor is rectangular or circular; a rectangular shell is selected when the operating pressure is normal pressure, and a circular shell is selected when the operating pressure is negative pressure or positive pressure; the inner sleeve is a prism, and the guide cones are all divergent guide cones. The guide cones in contact with the shell are prism divergent guide cones, and the guide cones not in contact with the shell are double-pyramid divergent guide cones; when the inner sleeve is a double-pyramid divergent guide cone, the inner sleeve is surrounded by a descending zone, and the inner sleeve and the inner sleeve adjacent to the horizontal direction are surrounded by an ascending zone; when the inner sleeve is a gap formed by two adjacent double-pyramid divergent guide cones, the inner sleeve is surrounded by an ascending zone, and the inner sleeve and the inner sleeve adjacent to the horizontal direction are surrounded by a descending zone; a regular filler for enhanced disturbance is arranged in the ascending zone.

7. The reactor according to claim 1 or 5, characterized in that The structured packing is plate mesh packing, model is 250X, 250Y, 350X, 350Y, 500X or 500Y.

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