CN215842896U - Continuous reactor suitable for high-viscosity high-solid-content reaction system - Google Patents

Abstract

The utility model relates to a continuous reactor suitable for high-viscosity high-solid-content reaction systems. The continuous reactor comprises a shell, a flow guide cone, an inner sleeve, a regular filler, a gas distributor and a hydrocyclone separator; the bottom in the reactor is provided with a gas distributor, the middle is provided with a guide cone and an inner sleeve, and the top of the reactor is provided with reaction internals such as a hydrocyclone and the like; 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 enables the fluid to contract inwards, and the divergence type flow guide cone enables the fluid to diverge outwards; regular packing is arranged in the inner part of the partial inner sleeve and the area surrounded by the partial inner sleeve and the shell; n M-level reaction levels are horizontally arranged in parallel in the reactor to obtain M-level N-level reactors, wherein M is less than or equal to 50, and N is less than or equal to 50; the utility model utilizes the multistage strong circulation field to better realize the mixing of solid and liquid materials and strengthen the reaction process, thereby improving the reaction conversion rate and the reaction rate.

Description

Continuous reactor suitable for high-viscosity high-solid-content reaction system

Technical Field

The utility model belongs to the field of chemical engineering reaction engineering, and particularly relates to a continuous reactor suitable for a high-viscosity high-solid-content reaction system.

Background

In the chemical reaction, the reaction process in which two different phases of liquid and solid exist simultaneously is called liquid-solid reaction, when the viscosity of reactants or products is greater than 100cp and the solid content is greater than 5%, the increase of the viscosity and the increase of solid particles hinder the probability of contact of the reactants and reduce the diffusion, heat transfer and mass transfer among the reactants, so that more time and energy consumption are required to obtain higher reaction conversion rate, and the reactions generally exist in the fields of petrifaction, coal chemical industry, medicine, pesticide, synthetic resin and the like.

In the industry, the reaction process of high viscosity and high solid content system mostly adopts a batch type mechanical stirring kettle, such as a reaction kettle in the production process of methyl isocyanate, aromatic polyamide and PTT fiber, and the batch type stirring kettle has the disadvantages and difficulties which are difficult to overcome, such as stirring effect brought by large-scale amplification, reaction heat transfer and the like, and especially has more strict requirements on the type of a stirring paddle when the material viscosity is higher.

The screw extruder is another choice of high-viscosity high-solid-content reaction system, particularly a double-screw reactor can process materials with higher viscosity, has high heat transfer efficiency and surface self-cleaning function, but the reaction residence time is not suitable for more than 0.5 hour, namely the high-viscosity high-solid-content reaction system with long reaction time still needs to be explored for other types of reactors.

Patent CN102416307B discloses an inner loop slurry bed reactor, sets up 1 ~ 160 built-in barrels in the reactor barrel, and every built-in barrel lower part is provided with gas distributor, and the continuous circulation of reaction liquid is flowed in the reactor, and this reactor has increased the quantity of inner tube in the barrel, has certain degree of difficulty when the handling capacity is great.

Patents CN1171667C and CN105400544A both propose a multistage loop reactor, which introduces a multistage form to benefit the high degree of upscaling, but the design of the reactor internals still has a serious defect that the multistage loop reactor cannot be applied to high-viscosity high-solid content reaction system because the inner sleeve is always a gas ascending region, which causes the short circuit of the materials, especially solid particle materials, in the inner sleeve and the inner wall region of the reactor, and has no recovery capability.

Therefore, the existing industrial reactor for treating the high-viscosity high-solid-content reaction system is still an intermittent stirring kettle, the intermittent reaction process needs to manually and frequently open the reaction kettle, toxic gas generated by side reaction in the production process is volatilized into the atmosphere, the environment and the safety of workers are influenced, parameters of the intermittent reaction process are large due to human factors and are not easy to control, and the product index is unstable or even unqualified. The utility model reduces the risk of material leakage and achieves intrinsic safety by inventing the continuous reactor suitable for the high-viscosity high-solid-content reaction system.

Disclosure of Invention

The utility model aims to provide a continuous reactor suitable for high-viscosity high-solid-content reaction systems, which can ensure that gas-liquid-solid three-phase systems are fully contacted, promote mixing, increase the contact area and the transfer coefficient of the interphase, strengthen mass transfer and heat transfer and improve the conversion rate. The reactor has the characteristics of low possibility of blockage, low energy consumption, large unit sectional area treatment capacity of the reactor, high conversion rate and the like.

The utility model provides a continuous reactor suitable for high-viscosity high-solid-content reactant systems, which mainly comprises a shell, a flow guide cone, an inner sleeve, regular packing, a gas distributor and a hydrocyclone separator. The reactor is mainly different from a batch reactor in that by arranging a reaction internal part and introducing inert gas, reactants are fully contacted under the action of the inert gas and the reaction internal part, the interphase contact area and the transfer coefficient are increased, the mass transfer and the heat transfer are enhanced, and the conversion rate is improved.

The technical scheme of the utility model is as follows:

a continuous reactor suitable for high-viscosity high-solid-content reaction systems is characterized by comprising a shell, a flow guide cone, an inner sleeve, regular packing, a gas distributor and a hydrocyclone separator; the bottom in the reactor is provided with a gas distributor, the middle is provided with a guide cone and an inner sleeve, and the top of the reactor is provided with reaction internals such as a hydrocyclone and the like; 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 enables the fluid to contract inwards, and the divergence type flow guide cone enables the fluid to diverge outwards; regular packing is arranged in the inner part of the partial inner sleeve and the area surrounded by the partial inner sleeve and the shell; the upper part of the gas distributor is a contraction type guide cone, the upper part of the gas distributor is an inner sleeve, the upper part of the gas distributor is a divergence type guide cone, the upper part of the gas distributor is an inner sleeve, the upper part of the gas distributor is an upper contraction type guide cone, and the upper contraction type guide cone is an upper hydrocyclone separator; the other mode is that the upper part of the gas distributor is provided with a divergent diversion cone, the upper part of the gas distributor is provided with an inner sleeve, a contractible diversion cone upwards is arranged upwards, an inner sleeve upwards is arranged upwards, a divergent diversion cone upwards is arranged upwards, and so on, the uppermost part of the gas distributor is provided with a hydrocyclone separator, structured packing is arranged inside the inner sleeve adjacent to the upper part of the contractible diversion cone no matter what arrangement mode, and structured packing is arranged in an area defined by the inner sleeve adjacent to the upper part of the divergent diversion cone and the shell.

The reactor shell is rectangular or circular, the inner sleeve is circular, and when the shell is rectangular, the divergent diversion cone and the convergent diversion cone are of a double-pyramid structure; when the shell is circular, the divergent diversion cone is of a biconical structure, and the convergent diversion cone is of a hollow cylindrical structure.

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

The inner sleeve of the reactor and the upper and lower adjacent guide cones form a reaction stage, and the reactor comprises a first-stage reaction stage, a second-stage reaction stage or a multi-stage reaction stage. The inner part of the inner sleeve adjacent to the upper part of the shrinkage type diversion cone forms a reaction level ascending area, regular packing is arranged in the reaction level ascending area, and the reaction level descending area is formed in the area surrounded by the inner sleeve and the shell; the region that divergent type water conservancy diversion awl upper portion adjacent inner skleeve and casing enclose forms the ascending district of reaction level, and this region sets up regular packing, and the inside decline district that forms the reaction level of inner skleeve.

N M-level reaction stages are horizontally arranged in parallel in the reactor to obtain M-level N-level reactors, M is less than or equal to 50, N is less than or equal to 50, and the cross sectional area between the inner sleeves in the horizontal direction is equal to that of the inner sleeves. The shell of the M-grade N-row reactor is rectangular or circular, the rectangular shell is preferred when the operating pressure is normal pressure, and the circular shell is preferred when the operating pressure is negative pressure or positive pressure; the inner sleeve is a frustum pyramid, the diversion cones are all divergent diversion cones, the diversion cone in contact with the shell is a frustum pyramid divergent diversion cone, and the diversion cone not in contact with the shell is a double-pyramid divergent diversion cone; when the lower part of the inner sleeve is provided with the biconical pyramid divergent diversion cones, the inner sleeve is internally surrounded into a descending area, the inner sleeve and the inner sleeve adjacent in the horizontal direction are surrounded into an ascending area, when the lower part of the inner sleeve is provided with a gap formed by two adjacent biconical pyramid divergent diversion cones, the inner sleeve is internally surrounded into an ascending area, and the inner sleeve adjacent in the horizontal direction are surrounded into a descending area; and regular packing for strengthening disturbance is arranged in the ascending area.

The structured packing is plate mesh packing with the model numbers of 250X, 250Y, 350X, 350Y, 500X and 500Y.

The operating temperature of the reactor is between normal temperature and 450 ℃, and the operating pressure is between 10kPa and 10 MPa.

The apparent flow velocity of the gas entering the reactor from the reactor is 0.01 m/s-1 m/s.

The inert gas introduced into the reactor may be any gas which does not chemically react with the reactants, preferably nitrogen.

The concrete description is as follows

A continuous reactor suitable for high-viscosity high-solid-content reactant system comprises a shell, a flow guide cone, an inner sleeve, regular packing, a gas distributor and a hydrocyclone separator; the bottom in the reactor is provided with a gas distributor, the middle is provided with a guide cone, an inner sleeve and regular fillers, and the top of the reactor is provided with reaction internals such as a hydrocyclone separator and the like; 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 enables fluid to contract inwards, and the divergence type flow guide cone enables the fluid to diverge outwards. Structured packing is arranged inside the partial inner sleeve and in the area enclosed by the partial inner sleeve and the shell. The upper part of the gas distributor is a contraction type guide cone, the upper part of the gas distributor is an inner sleeve, the upper part of the gas distributor is a divergence type guide cone, the upper part of the gas distributor is an inner sleeve, the upper part of the gas distributor is an upper contraction type guide cone, and the upper contraction type guide cone is an upper hydrocyclone separator; the second mode is that the upper portion of gas distributor is for dispersing type water conservancy diversion awl, and its upper portion is the inner skleeve, upwards again for contracting type water conservancy diversion awl, upwards again for inner skleeve, upwards again for dispersing type water conservancy diversion awl, analogizes from this, and the top is hydrocyclone separator, no matter what kind of arrangement, and contracting type water conservancy diversion awl upper portion adjacent inner skleeve is inside to be set up regular packing, and the region that adjacent inner skleeve and the casing in dispersing type water conservancy diversion awl upper portion enclose sets up regular packing.

The inner sleeve, the regular packing and the upper and lower adjacent guide cones form a reaction stage, and the reactors are divided into a first-stage reactor, a second-stage reactor or a multi-stage reactor according to the number of the reactors arranged on the inner sleeve in the vertical direction. The simplest structure of the first-stage reactor is that a gas distributor, a contraction type diversion cone, an inner sleeve, regular fillers, a divergence type diversion cone and a hydrocyclone separator are arranged from bottom to top according to a first arrangement mode; according to a second arrangement mode, the gas distributor, the divergent diversion cone, the inner sleeve, the regular filler, the contraction diversion cone and the hydrocyclone separator are arranged from bottom to top. The inner sleeve adjacent to the upper part of the shrinkage type diversion cone forms a reaction level ascending area, regular packing for enhancing disturbance is arranged in the reaction level ascending area, and the reaction level descending area is formed by the area surrounded by the inner sleeve and the shell; the region enclosed by the inner sleeve and the shell adjacent to the upper part of the divergent diversion cone forms an ascending region of the reaction level, the region is also provided with regular packing for strengthening, and a descending region of the reaction level is formed inside the inner sleeve. The second-stage reactor is formed by adding an inner sleeve, regular packing and a diversion cone on the basis of the first-stage reactor, and specifically, the inner sleeve, the regular packing and a contraction type diversion cone are added on the upper part of the divergence type diversion cone on the inner sleeve of the first-stage reactor in a first arrangement mode, or the inner sleeve, the regular packing and the divergence type diversion cone are added on the upper part of the contraction type diversion cone on the inner sleeve of the first-stage reactor in a second arrangement mode. The number of the inner cylinder bodies of the reactor in the vertical direction is 2, wherein the inner sleeves and the regular packing which are close to the lower positions form a first reaction stage together with the guide cones which are adjacent to the upper and lower positions of the inner sleeves and the regular packing which are close to the upper positions form a second reaction stage together with the guide cones which are adjacent to the upper and lower positions of the inner sleeves, and the guide cones between the two inner sleeves are the common part of the first reaction stage and the second reaction stage. And the like, when 3 or more inner sleeves and corresponding flow guide cones are arranged in the vertical direction, a three-stage or multi-stage reactor is formed.

N M-level reaction levels are arranged in parallel in the reactor to obtain M-level N-level reactors, M is less than or equal to 50, N is less than or equal to 50, and the cross sectional area between the inner sleeves in the horizontal direction is equal to that of the inner sleeves. The shell of the M-grade N-row reactor is rectangular or circular, the rectangular shell is preferred when the operating pressure is normal pressure, and the circular shell is preferred when the operating pressure is negative pressure or positive pressure; the inner sleeve is a frustum pyramid, the diversion cones are all divergent diversion cones, the diversion cone in contact with the shell is a frustum pyramid divergent diversion cone, and the diversion cone not in contact with the shell is a double-pyramid divergent diversion cone; when the lower part of the inner sleeve is provided with the biconical pyramid divergent diversion cones, the inner sleeve is internally surrounded into a descending area, the inner sleeve and the inner sleeve adjacent in the horizontal direction are surrounded into an ascending area, when the lower part of the inner sleeve is provided with a gap formed by two adjacent biconical pyramid divergent diversion cones, the inner sleeve is internally surrounded into an ascending area, and the inner sleeve adjacent in the horizontal direction are surrounded into a descending area; and regular packing for strengthening disturbance is arranged in the ascending area.

A continuous reactor suitable for high-viscosity high-solid content reaction system is composed of gas inlet, upper and lower inlets, upper and lower outlets, and gas outlet.

The reactor shell is rectangular or round, and when the shell is rectangular, the divergent diversion cone and the convergent diversion cone are of a double-pyramid structure; when the shell is circular, the divergent diversion cone is of a biconical structure, and the convergent diversion cone is of a hollow cylindrical structure.

Taking a first stage reactor, a first arrangement as an example, the flow of the reactor liquid and solids when the reaction mass is bottom in and top out is as follows: one or more reaction materials enter the bottom of the reactor from a feed inlet at the lower part of the reactor, gas enters the reactor from a gas inlet at the bottom of the reactor, the reaction liquid at the bottom of the tower is disturbed after being distributed by a gas distributor, the mixing of the reaction liquids is strengthened, the reaction liquids move upwards, the gas flow rate at the center of the shrinkage type diversion cone is far greater than that at the edge of the shrinkage type diversion cone, so the liquid-solid reaction liquid is carried by the gas to move upwards at the center of the shrinkage type diversion cone, the liquid-solid reaction liquid moves downwards at the edge of the shrinkage type diversion cone, and then is carried by the rising gas to move upwards from the center of the shrinkage type diversion cone, namely the liquid-solid reaction liquid completes a circular flow at the shrinkage type diversion cone; the liquid-solid reaction liquid from the contraction type guide cone continuously moves upwards and enters an ascending area in the inner sleeve, the divergence type guide cone on the upper portion of the inner sleeve prevents the reaction liquid from continuously moving upwards, the liquid-solid reaction liquid moves upwards obliquely to the farthest position of the guide cone along the lower cone surface of the divergence guide cone, a part of the liquid-solid reaction liquid is affected by gravity, a small amount of gas is entrained to enter a descending area outside the inner sleeve, the contraction type guide cone prevents the part of the reaction liquid from continuously descending, the liquid-solid reaction liquid moves downwards obliquely along the upper inclined surface of the contraction guide cone, 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, and therefore second circulation flow is completed inside and outside the inner sleeve; at the center of the divergent diversion cone and the shell, the liquid-solid reaction liquid is carried by the gas to enter the upper part of the divergent diversion cone, and at the edge of the divergent diversion cone and the shell, because the gas amount is less, part of the liquid-solid reaction liquid moves downwards from the upper part of the divergent diversion cone and is carried by the gas to the upper part of the divergent diversion cone again, so that the liquid-solid reaction liquid completes a circular flow at the divergent diversion cone again. The circular flow strengthens the mixing of gas phase, liquid phase and solid phase, increases the contact probability of reactants, improves the reaction rate, and discharges the liquid-solid reaction liquid from a discharge hole at the upper part of the reactor after the reaction is finished; the gas is discharged from a gas outlet at the top of the reactor after separating entrained liquid and solids when passing through the hydrocyclone separator.

Taking a first-stage reactor as an example, the first arrangement is that when the reaction materials are fed in and discharged out, the flow of the fluid in the reactor is as follows: one or more reaction materials enter the upper area of the divergent diversion cone from a feed inlet at the upper part of the reactor, partial liquid-solid reaction liquid moves downwards from the upper part of the divergent diversion cone at the edge of the divergent diversion cone and the shell due to less gas flow, and the liquid-solid reaction liquid is carried by a large amount of gas to enter the upper part of the divergent diversion cone at the center of the divergent diversion cone and the shell, so that the liquid-solid reaction liquid completes a circular flow between the divergent diversion cone and the shell. The liquid-solid reaction liquid from the divergent diversion cone and the shell continuously moves downwards and enters a descending area outside the inner sleeve, the convergent diversion cone prevents the reaction liquid from continuously descending, the liquid-solid reaction liquid moves downwards along the upper inclined plane of the convergent diversion cone and is carried into an ascending area inside the inner sleeve by a large amount of gas from the center of the convergent diversion cone, the divergent diversion cone on the upper part of the inner sleeve prevents the reaction liquid from continuously moving upwards, the liquid-solid reaction liquid moves upwards along the lower conical plane of the divergent diversion cone to the farthest position of the diversion cone, and a part of the liquid-solid reaction liquid is acted by gravity and a small amount of gas is entrained to enter the descending area outside the inner sleeve, so that a second circular flow is completed inside and outside the inner sleeve; the central gas flow velocity of the shrinkage type guide cone is far greater than the edge of the shrinkage type guide cone, so that the liquid-solid reaction liquid is carried by gas to move upwards in the center of the shrinkage type guide cone, the liquid-solid reaction liquid moves downwards in the edge of the shrinkage type guide cone and is carried by the rising gas to move upwards from the center of the shrinkage type guide cone, namely the liquid-solid reaction liquid completes a circular flow again in the shrinkage type guide cone; the circular flow strengthens the mixing of gas phase, liquid phase and solid phase, increases the contact probability of reactants, improves the reaction rate, and discharges the liquid-solid reaction liquid from a discharge hole at the lower part of the reactor after the reaction is finished; the gas is discharged from a gas outlet at the top of the reactor after separating entrained liquid and solids when passing through the hydrocyclone separator.

N M-level reaction stages are horizontally arranged in parallel in the reactor to obtain M-level N-level reactors, M is less than or equal to 50, N is less than or equal to 50, and the cross sectional area between the inner sleeves in the horizontal direction is equal to that of the inner sleeves. The shell of the M-grade N-row reactor is rectangular or circular, the rectangular shell is preferred when the operating pressure is normal pressure, and the circular shell is preferred when the operating pressure is negative pressure or positive pressure; the inner sleeve is a frustum pyramid, the diversion cones are all divergent diversion cones, the diversion cone in contact with the shell is a frustum pyramid divergent diversion cone, and the diversion cone not in contact with the shell is a double-pyramid divergent diversion cone; when the lower part of the inner sleeve is provided with the biconical pyramid divergent diversion cones, the inner sleeve is internally surrounded into a descending area, the inner sleeve and the inner sleeve adjacent in the horizontal direction are surrounded into an ascending area, when the lower part of the inner sleeve is provided with a gap formed by two adjacent biconical pyramid divergent diversion cones, the inner sleeve is internally surrounded into an ascending area, and the inner sleeve adjacent in the horizontal direction are surrounded into a descending area; and regular packing for strengthening disturbance is arranged in the ascending area.

The utility model has the advantages that:

the disturbance of gas and the density difference inside and outside the inner sleeve make the gas-liquid-solid three-phase matter contact fully, promote mixing, increase the interphase contact area and transfer coefficient, strengthen mass transfer and heat transfer and reach high conversion rate.

The solid particles are uniformly distributed in the reactor, local accumulation or deposition cannot occur, the treatment capacity of the unit sectional area of the reactor is large, and the industrial amplification is easy.

The reaction materials flow in the ascending area and the descending area and between the guide cones in a directional and circular way, the materials on the surfaces of the reactor and the inner sleeve are continuously updated, the temperature distribution is uniform, and the reactor is particularly suitable for exothermic reaction

The utility model utilizes the multistage strong circulation field to better realize the mixing of solid and liquid materials and strengthen the reaction process, thereby improving the reaction conversion rate and the reaction rate.

Drawings

FIG. 1 is a schematic diagram of a continuous first stage reactor for high viscosity high solids reaction systems

FIG. 2 is a schematic diagram of a continuous two-stage reactor for high viscosity high solids reaction systems

FIG. 3 is a schematic view of a retractable guide cone

FIG. 4 is a schematic view of a divergent flow cone

FIG. 5 Structure of a continuous 3-stage 3-series reactor for high viscosity high solids reaction systems

FIG. 6 is a schematic diagram of a continuous M-stage N-series reactor for high viscosity high solids reaction systems

Wherein: 1-shell, 2-contraction type diversion cone, 3-inner sleeve, 4-divergence type diversion cone, 5-regular packing, 6-gas distributor, 7-cyclone, 8-gas inlet, 9-lower part feed inlet, 10-lower part discharge outlet, 11-upper part feed inlet, 12-upper part discharge outlet and 13-gas outlet.

Detailed Description

The utility model is described in further detail below with reference to the accompanying drawings:

example 1

Example 1 is the use of a continuous first stage reactor for the synthesis of 2-amino-8-naphthol-6-sulfonic acid as a high viscosity high solids reaction system.

As shown in fig. 1, 3 and 4:

the reactor comprises a shell 1, a contraction type diversion cone 2, an inner sleeve 3, a divergence type diversion cone 4, a regular packing 5, a gas distributor 6 and a hydrocyclone 7; the reactor internal parts comprise a gas distributor 6, a contraction type diversion cone 2, an inner sleeve 3, a regular filler 5, a divergence type diversion cone 4 and a hydrocyclone separator 7 from bottom to top; the reactor is provided with a gas inlet 8, an upper feed inlet 11, an upper discharge outlet 12, a lower feed inlet 9, a lower discharge outlet 10 and a gas discharge outlet 13. The lower diversion cone of the inner sleeve 3 is a contraction diversion cone 2, the inner sleeve 3 is a rising area, and the outer sleeve 3 is a falling area; structured packing 5 for enhancing turbulence is arranged in the rising zone.

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 diversion cone 2 or the divergence type diversion cone 4 accounts for 20% of the area of the inner sleeve 3, the gap area between the contraction type diversion cone 2 accounts for 25% of the area of the inner sleeve 3, and the gap area between the divergence type diversion cone 4 and the shell 1 accounts for 25% of the area of the inner sleeve. The regular packing 5 adopts 350X plate net packing; the reactor shell 1 is circular, the contraction type guide cone 2 adopts a hollow cylinder structure as shown in figure 3, and the divergence type guide cone 4 adopts a double-cone structure as shown in figure 4.

The synthesis effect of the reactor applied to 2-amino-8-naphthol-6-sulfonic acid is as follows: heating a 2-naphthylamine-6, 8-disulfonic acid solution, potassium hydroxide and sodium hydroxide in a raw material premixing tank according to the molar ratio of 1:1:1 to 180 ℃, and stirring until the solution is molten; the premixed liquid enters the reactor through a raw material inlet at the lower part of the reactor at the flow rate of 25 kg/h; nitrogen gas with the temperature of 200 ℃ enters the reactor from the bottom of the reactor, and the apparent flow velocity of the nitrogen gas in the reactor is 0.2 m/s; the viscosity of the reaction system is 200cp, and the reaction temperature of the reactor is controlled to 200 +/-5 ℃ by a jacket; the reaction pressure is controlled to be between 0.3 plus or minus 0.05MPa through a regulating valve for controlling the gas phase at the top of the reactor; the reaction time is 2h, and the reaction solution after the reaction is finished flows into a product buffer tank from a product outlet at the upper part of the reactor by adding water, is diluted and cooled and then enters an acid precipitation process; and removing carried ammonia gas and phenolic impurities from the gas phase at the top of the reactor through a gas washing tank, and discharging nitrogen at a high point after absorbing waste gas. After the product is acidified and filtered, 98.66% of 2-amino-8-naphthol-6-sulfonic acid and 0.06% of 2-naphthylamine-6, 8-disulfonic acid are analyzed by liquid chromatography. Compared with a batch kettle type reactor, the reactor shortens the reaction residence time, has the product temperature, and is easy to amplify.

Example 2

Example 2 is the use of a continuous two stage reactor with a high viscosity high solids reaction system for the synthesis of methyl isocyanate.

As shown in fig. 2, 3 and 4:

the reactor comprises a shell 1, a contraction type diversion cone 2, an inner sleeve 3, a divergence type diversion cone 4, a regular packing 5, a gas distributor 6 and a hydrocyclone 7; the reactor internal parts comprise a gas distributor 6, a contraction type diversion cone 2, an inner sleeve 3, a regular filler 5, a divergence type diversion cone 4 and a hydrocyclone separator 7 from bottom to top; the reactor is provided with a gas inlet 8, an upper feed inlet 11, an upper discharge outlet 12, a lower feed inlet 9, a lower discharge outlet 10 and a gas discharge outlet 13. The lower diversion cone of the lower position in the two inner sleeves 3 is a contraction type diversion cone 2, the inner sleeve 3 is internally provided with a rising area, the outer part of the inner sleeve 3 is a falling area, the lower diversion cone of the higher position in the two inner sleeves 3 is a divergence type diversion cone 4, the outer part of the inner sleeve 3 is a rising area, the inner part of the inner sleeve 4 is a falling area, and all rising areas are internally provided with regular packing 5 for strengthening disturbance.

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 diversion cone 2 or the divergence type diversion cone 4 accounts for 25% of the area of the inner sleeve 3, the gap area between the contraction type diversion cone 2 accounts for 250% of the area of the inner sleeve 3, and the gap area between the divergence type diversion cone 4 and the shell 1 accounts for 20% of the area of the inner sleeve. The regular packing 5 adopts 250X plate net packing; the reactor shell 1 is rectangular, the contraction type guide cone 2 adopts a double-pyramid structure as shown in figure 3, the divergence type guide cone 4 adopts a double-pyramid structure as shown in figure 4,

the reactor has the following synthesis effect on methyl isocyanate:

180# solvent oil enters the reactor through a feed inlet at the lower part of the reactor at the flow rate of 2000g/h, 267g/h of sodium cyanate and 323g/h of dimethyl sulfate, the solid content of the reaction system is 28%, and the reaction temperature is controlled at 180 ℃ by a jacket; nitrogen gas with the temperature of 180 ℃ enters the reactor from the bottom of the reactor, and the apparent flow velocity of the nitrogen gas in the reactor is 0.43 m/s; the reaction is kept for 2 hours, other materials after the reaction are extracted from a material outlet at the upper part of the reactor, and 189g/h of methyl isocyanate is obtained by condensing and separating nitrogen and the generated methyl isocyanate; the content of methyl isocyanate was 99.5% by chromatography. The reactor is used for making the synthesis of methyl isocyanate become continuous operation, reducing the risk of high-toxicity gas leakage, improving the operation environment and improving the intrinsic safety of the process.

Example 3

Example 3 is the use of a three-stage three-column reactor with continuity of a high viscosity high solids reaction system for the synthesis of 2, 4-dichlorophenoxyacetic acid from sodium 2, 4-dichlorophenolate and sodium chloroacetate.

As shown in fig. 6:

m is less than or equal to 50, N is less than or equal to 50, and the cross-sectional area between the inner sleeves 3 in the horizontal direction is equal to that of the inner sleeves 3. The shell 1 of the M-level N-row reactor is rectangular or circular, the rectangular shell is preferred when the operating pressure is normal pressure, and the circular shell is preferred when the operating pressure is negative pressure or positive pressure; the inner sleeve 3 is a frustum pyramid, the diversion cones are all divergent diversion cones 4, the diversion cone in contact with the shell is the frustum pyramid divergent diversion cone 4, and the diversion cone not in contact with the shell is the double-pyramid divergent diversion cone 4; when the lower part of the inner sleeve 3 is a double-pyramid divergent diversion cone 4, a descending area is defined by the inner part of the inner sleeve 3, an ascending area is defined by the inner sleeve 3 and the inner sleeve 3 adjacent to each other in the horizontal direction, when a gap formed by two adjacent double-pyramid divergent diversion cones 4 is formed by the lower part of the inner sleeve 3, an ascending area is defined by the inner part of the inner sleeve, and a descending area is defined by the inner sleeve 3 and the inner sleeve 3 adjacent to each other in the horizontal direction; the regular packing 5 for strengthening disturbance is arranged in the ascending area.

As shown in fig. 3, 4, and 5:

selecting M, N as three-stage three-column reactors from M-stage N-column reactors; comprises a shell 1, a contraction type diversion cone 2, an inner sleeve 3, a divergence type diversion cone 4, a regular packing 5, a gas distributor 6 and a hydrocyclone 7; the reactor internals include a gas distributor 6, a divergent diversion cone 4 or the left part and the right part thereof, an inner sleeve 3, a regular packing 5, a divergent diversion cone 4 and a hydrocyclone separator 7 from bottom to top; the reactor is provided with a gas inlet 8, an upper feed inlet 11, an upper discharge outlet 12, a lower feed inlet 9, a lower discharge outlet 10 and a gas discharge outlet 13. Two inner sleeves 3 at the lower left and upper and lower divergent diversion cones 4 thereof are the second-stage reactor of the embodiment 2, a third-stage reactor is obtained by adding one inner sleeve 3, regular packing 5 and divergent diversion cone 4 on the basis of the embodiment 2, a third-stage three-row reactor is obtained by arraying the third-stage reactor in the horizontal direction twice, and the cross sectional area between the inner sleeves 3 in the horizontal direction is equal to that of the inner sleeves 3.

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 diversion cone 4 accounts for 25% of the area of the inner sleeve 3, the gap area between the convergent diversion cone 2 accounts for 25% of the area of the inner sleeve 3, and the gap area between the divergent diversion cone 4 and the shell 1 accounts for 15% of the area of the inner sleeve. The regular packing 5 adopts 500X plate net packing; the reactor shell 1 is rectangular, and the divergent guide cone 4 adopts a double-pyramid divergent guide cone and a frustum-pyramid divergent guide cone as shown in fig. 4.

Industrially, 2, 4-dichlorophenoxyacetic acid is synthesized by 2, 4-dichlorophenolate sodium salt and sodium chlorate in an intermittent kettle type reactor, the solid content of a reaction system is 30 percent, a discharge port of the intermittent kettle type reactor with 5 kettles connected in series is easy to block, the yield of a device is influenced, and the effects of three-stage three-row continuous reactors adopting the high-viscosity high-solid content reaction system of the utility model are as follows:

the molar ratio of the 2, 4-dichlorophenol sodium salt to the sodium chlorate is 1.1:1, the sodium chlorate enters the reactor through a feed inlet at the upper part of the reactor, the solid content of the reaction system is 30 percent, and the reaction temperature is controlled at 110 ℃ by a jacket; nitrogen gas with the temperature of 110 ℃ enters the reactor from the bottom of the reactor, and the apparent flow velocity of the nitrogen gas in the reactor is 0.28 m/s; when the reaction retention time is 6%, nitrogen is extracted from a material outlet at the upper part of the reactor, a solid-liquid mixture is extracted from a material outlet at the lower part of the reactor, and the conversion rate of the 2, 4-dichlorophenol sodium is 91% by analysis. The reactor makes the production of 2, 4-dichlorophenoxyacetic acid be continuous and stable operation, avoids the unplanned shutdown caused by the blockage of the discharge port of the intermittent kettle, and replaces 5 intermittent kettles connected in series with one vertical reactor, thereby greatly reducing the floor area of the device.

The above embodiments are merely preferred examples to illustrate the present invention, and it should be apparent to those skilled in the art that any obvious variations and modifications can be made without departing from the spirit of the present invention.

Claims (7)

1. A continuous reactor suitable for high-viscosity high-solid-content reaction systems is characterized by comprising a shell, a flow guide cone, an inner sleeve, regular packing, a gas distributor and a hydrocyclone separator; the bottom in the reactor is provided with a gas distributor, the middle is provided with a guide cone and an inner sleeve, and the top of the reactor is provided with a hydrocyclone separation internal part; 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 enables the fluid to contract inwards, and the divergence type flow guide cone enables the fluid to diverge outwards; regular packing is arranged in the inner sleeves adjacent to the upper part of the contraction type guide cone, and the regular packing is arranged in the area surrounded by the inner sleeves adjacent to the upper part of the divergence type guide cone and the shell; the upper part of the gas distributor is a contraction type guide cone, the upper part of the gas distributor is an inner sleeve, the upper part of the gas distributor is a divergence type guide cone, the upper part of the gas distributor is an inner sleeve, the upper part of the gas distributor is an upper contraction type guide cone, and the upper contraction type guide cone is an upper hydrocyclone separator; in another mode, the upper part of the gas distributor is a divergent diversion cone, the upper part of the gas distributor is an inner sleeve, the upper part of the gas distributor is a contraction diversion cone, the upper part of the gas distributor is an inner sleeve, the upper part of the gas distributor is a divergent diversion cone, the upper part of the gas distributor is an inner sleeve, the upper part of the gas distributor is an upward divergent diversion cone, the uppermost part of the gas distributor is a hydrocyclone.

2. A continuous reactor suitable for use with high viscosity and high solids reactant systems as in claim 1, wherein the reactor shell is rectangular or circular, and when the shell is rectangular, the divergent and convergent deflector cones are in the form of a double pyramid; when the shell is circular, the divergent diversion cone is of a biconical structure, and the convergent diversion cone is of a hollow cylindrical structure.

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

4. The reactor of claim 1, wherein the inner sleeve of the reactor and the upper and lower adjacent guide cones form a reaction stage, and the reactor comprises a first-stage reaction stage, a second-stage reaction stage or a multi-stage reaction stage; the inner part of the inner sleeve adjacent to the upper part of the shrinkage type diversion cone forms a reaction level ascending area, regular packing is arranged in the reaction level ascending area, and the reaction level descending area is formed in the area surrounded by the inner sleeve and the shell; the region that divergent type water conservancy diversion awl upper portion adjacent inner skleeve and casing enclose forms the ascending district of reaction level, and this region sets up regular packing, and the inside decline district that forms the reaction level of inner skleeve.

5. The reactor as claimed in claim 1, wherein M reaction stages are arranged in parallel N times, M is less than or equal to 50, N is less than or equal to 50, and the cross-sectional area between the inner sleeves in the horizontal direction is equal to that of the inner sleeves.

6. The reactor of claim 5 wherein the shell of the M-stage N-row reactor is rectangular or circular; selecting a rectangular shell when the operating pressure is normal pressure, and selecting a circular shell when the operating pressure is negative pressure or positive pressure; the inner sleeve is a frustum pyramid, the diversion cones are all divergent diversion cones, the diversion cone in contact with the shell is a frustum pyramid divergent diversion cone, and the diversion cone not in contact with the shell is a double-pyramid divergent diversion cone; when the lower part of the inner sleeve is provided with the biconical pyramid divergent diversion cones, the inner sleeve is internally surrounded into a descending area, the inner sleeve and the inner sleeve adjacent in the horizontal direction are surrounded into an ascending area, when the lower part of the inner sleeve is provided with a gap formed by two adjacent biconical pyramid divergent diversion cones, the inner sleeve is internally surrounded into an ascending area, and the inner sleeve adjacent in the horizontal direction are surrounded into a descending area; and regular packing for strengthening disturbance is arranged in the ascending area.

7. The reactor of claim 1 or 5, wherein the structured packing is trawl packing of type 250X, 250Y, 350X, 350Y, 500X or 500Y.

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