JP3323213B2 - Reaction method of suspension catalyst system - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to the use of cross-flow filtration as a catalyst separation system in producing a liquid reaction product by a chemical reaction between a liquid and a liquid or a liquid and a gas in a fluidized catalyst suspension bed. Thus, the present invention relates to a reaction method characterized in that a liquid reaction product from which a catalyst has been separated is stably withdrawn continuously for a long period of time.

[0002]

2. Description of the Related Art In the chemical industry, a solid-liquid phase or a gas-liquid-solid three-phase reaction system using a solid catalyst includes a reaction method using a fixed-bed system or a fluidized-bed catalyst suspension system. The fixed bed type reaction method has an advantage that the catalyst can be easily separated, and the reaction can be performed while maintaining the catalyst at a high concentration. However, in order to keep the catalyst fixed in the reactor, not to increase the pressure loss due to the filled catalyst, and to secure the required reaction active point, the catalyst is in the form of pellets with fine pores or large particle size. You need to use Therefore, for example, in a reaction where catalyst poisoning is severe, activity degradation on the catalyst surface is large, and active points inside the catalyst may not be used. In addition, the reaction having a low mass transfer rate in the pores of the catalyst has a drawback that the reaction on the surface of the catalyst is mainly performed, so that the utilization efficiency of the catalyst is low. Further, in a system involving reaction heat, it is difficult to control the temperature, and there is a problem that an abnormal reaction, permanent poisoning of the catalyst, and the like occur due to generation of a hot spot or the like.

[0003] In order to solve these problems, a slurry reaction using a suspended catalyst having a smaller particle size of the catalyst than in the case of a fixed bed may be considered. That is, the catalyst suspension fluidized bed system is a reaction device that performs a reaction by improving the mixing and interphase contact including the catalyst and the liquid and, in some cases, the gas, using a stirring tank, a gas lift, a circulation pump, etc., and a reaction solution slurry. It consists of a catalyst separation device that separates the catalyst and the reaction solution.
For example, when a sedimentation separator (4) as shown in FIG. 4 is used as this catalyst separation apparatus, the apparatus becomes excessive due to the sedimentation speed caused by the specific gravity difference of the solid-liquid of the system, the catalyst particle diameter, etc. the system is Ru limited. Further, when the particle size is fine, it is very difficult to completely separate the catalyst, and the catalyst is mixed into the reaction product, which is a filtrate, and there are problems such as clogging and scaling in the subsequent process and catalyst loss. . In addition, mechanical separators such as centrifugal separators may not be applicable to high pressure systems and systems handling hazardous materials due to their sliding and sealing parts. Therefore, there is a problem that the separation performance is reduced and the catalyst is mixed into the filtrate.

[0004] In order to solve these problems, when a differential pressure type filter filter is used in the catalyst separation device, it is possible to reliably separate even the fine particles having a particle diameter of the order of microns on the catalyst. Thereby, an improvement in the reaction rate can be expected. However, frequent backwashing must be performed due to filter clogging and scaling, etc., and a decrease in filtration speed. Here, back washing means that the filtrate or gas flows into the filtration surface in the opposite direction to the time of filtration, that is, from the filtrate side, and cleans solid clogs and cake on the slurry side of the filter to regenerate filtration performance. It is.

[0005] As a result, when the filtrate is used for back washing, the separated filtrate is returned to a slurry, which is inefficient. When a gas is used for back washing, disturbance is given to the reaction system. Since the operation of the system must be stopped at the time of cleaning, there is a problem that stable and smooth continuous operation cannot be performed. As described in JP-B-55-49538, especially for highly concentrated slurries (3% by weight or more), a filter medium made of a material having low flexibility such as ceramic or sintered metal is used . When used, there is a problem that the filtration rate decreases with time, and the effect of backwashing to improve the recovery rate of the filtration rate is small.

[0006]

SUMMARY OF THE INVENTION Accordingly, the present inventors
According to the patent publication, an experiment of ethylbenzene synthesis by benzene alkylation was conducted in a reactor having a filter using a flexible filter. Here, a stainless steel wire mesh was used for the filter due to the solvent resistance to benzene (5 μm with a minimum aperture).
As a result, the recovery of the filtration rate by the backwash was certainly good. However, the backwashing cycle is about 24 hours due to a decrease in filtration rate, the reaction system is disturbed by the backwashing, the operation is unstable and complicated, and the mesh size is 5 microns and the particle size is smaller than this. There is a problem that the catalyst flows out. An object of the present invention is to solve these problems.

[0007]

In order to solve the above-mentioned problems, the present inventors have conducted a continuous reaction / catalyst separation on a catalyst slurry by using various filter media of ceramic or sintered metal having a fine pore diameter. The research was advanced on how to do it smoothly. As a result, they have found that the reaction system using the cross-flow filtration works well.

That is, the present invention relates to a method for obtaining a liquid reaction product by a liquid-liquid or liquid-gas contact reaction in the presence of a particulate solid catalyst. (2) a slurry concentration of 3 weight mainly composed of a liquid reaction product
% Or more of a catalyst suspension using a filter medium having an average pore diameter of 0.5 to 10 μm, and a cross flow linear velocity of 0.05 m
Separating the liquid reaction product and the concentrated catalyst suspension by filtration in a cross-flow system at a rate of not less than 3 g / sec. (3) circulating the concentrated catalyst suspension to a suspension fluidized bed It is a continuous reaction method characterized by having.

Here, the cross-flow filtration means a pressure difference between the slurry (suspension) side and the filtrate side across a filter medium (filter) (the pressure difference at this time is referred to as a filtration differential pressure; the same applies hereinafter). Filtration is performed using this as a driving force, and the slurry is continuously filtered while the slurry flows parallel to the filtration surface (the average flow velocity per cross-sectional area of the slurry at this time is referred to as a cross-flow linear velocity: the same applies hereinafter). Is what you do. For example, when a tubular filter is used, a method is used in which the slurry extracted from the reactor is supplied from one of the filter tubes, the concentrated slurry is discharged from the other of the filter tubes, and the filtrate is separated through the filter tube filtration surface.
However, this filter tube has a filtering surface on the whole or a part of the tube wall surface, and the cross-sectional shape of the tube is not limited to a circular shape. Further, the slurry may be inside the filter tube and the filtrate may be inside the filter tube.

In the cross-flow filtration used in the present invention, the growth of a solid cake of the slurry on the filtration surface is suppressed by the shearing force of the slurry flowing parallel to the filtration surface, and the filtration rate decreases with time. Suppress. This eliminates the need for intermittent backwashing and enables continuous operation. The average particle diameter (including the hydraulic equivalent diameter) of the secondary particles of the catalyst is not particularly limited, but a catalyst having a particle diameter of 1 mm or less is preferable. Here, the secondary particle is an aggregate of the primary particle with respect to the primary particle which is the minimum unit of the solid particle. In general, reducing the particle diameter has the advantage of increasing the reaction rate by increasing the surface area (specific surface area) per unit volume of the catalyst and increasing the effective active sites. However, the particle size must be such that the catalyst does not flow through the pores of the filter medium.

The concentration of the slurry may be in a range that allows handling, for example, a range in which there is no clogging or settling of solids in the piping. At low concentrations, conventional differential pressure filters are sufficiently stable for filtration, and the backwashing cycle can be lengthened. However, when the concentration is higher than 3% by weight, the present reaction system has a stable filtration rate and a backwashing cycle. Very effective in prolonging

[0012] The viscosity of the slurry may be in the range in which it can flow. There is no particular problem in the low viscosity region up to about 100 cP (centipoise), but in the fluid in the high viscosity region, the pressure difference between the inlet and the outlet of the slurry filter (pressure loss at the filter wall) and the filtration pressure difference increase. In some cases, clogging of the solids in the piping may occur, or the rate of withdrawing the filtrate from the filter may become extremely slow due to a decrease in the fluidity of the liquid. Here, the upper limit of the slurry viscosity differs depending on the characteristics and purpose of the system and cannot be uniquely limited.

[0013] pore diameter of the filter of the filter medium, the basic, although it comes to may be used smaller than the minimum catalyst diameter, however, the definition of the minimum diameter of the catalyst also problems such as measurement accuracy Difficult to include. Even when the pore size of the filter medium is larger than the minimum catalyst particle size, bridging or cake formation may cause few particles to pass through the cake (cake filtration).

Further, the inventors have found that the suspended catalyst is a stirring blade,
By mechanical pulverization by collision of the solid catalyst with a circulation pump, piping, etc., it was confirmed that fine particles considerably smaller than the initial average particle diameter were generated, and the fine particles were clogged in the filter, causing a reduction in filtration speed. Therefore, as a result of further research using various types of suspension catalysts, this atomization is almost stable at a constant value (this is because the dispersion and agglomeration of particles are balanced and the energy required for atomization is reduced). It is considered that the smaller the particle size, the larger the size.) That is, about 2 to 5% by weight of particles having a small particle size in the integrated particle size distribution showed little change with time such as further atomization or increase. Furthermore, this stable particle size is 0.5
It has been found that catalyst separation can be performed smoothly without clogging by using a filter medium having a pore size of about 10 to about 10 microns.

The tube diameter of the cross section of the filter medium on the slurry side of the filter, or the minimum gap of a flat plate, is preferably 3 mm or more and 100 mm or less. This is because if the size is smaller than 3 mm, clogging of the slurry occurs, and stable operation is difficult, and regeneration of the filtration capacity becomes impossible. When the size is larger than 100 mm, it is difficult to obtain a large filtration area. That is, even if the filtration area is the same, the larger the size is, the larger the filtering device becomes.

In a cross-flow filter, the linear velocity of the slurry in order to apply a shearing force to the slurry flowing on the filtration surface depends on the slurry concentration of the system, viscosity, catalyst particle diameter, filter diameter of the filter, and the like. 0.05m / s (m / s
Second: the same applies hereinafter) or more, preferably 0.1 to 20 m /
s. When the slurry linear velocity is increased, the shearing force increases and the cake thickness decreases, so the filtration rate increases.However, the pressure difference between the inlet and outlet of the slurry passing through the filter increases, and the power required for slurry circulation increases. turn into. Conversely, if the slurry linear velocity is less than 0.05 m / s, the shearing force will be small, the cake thickness will be large, and the filtration speed will be small.

[0017] The filtration differential pressure in the cross flow filter is 20K
g / cm ² or less, preferably 0.05 to 10 kg /
cm ² . The filtration pressure difference is approximately proportional to the filtration speed if the cake thickness is constant. However, when the filtration pressure difference is excessively increased to increase the filtration speed, the adhesion of the cake to the filtration surface increases, and at the same slurry linear velocity, the thickness of the cake increases due to the balance between the adhesion to the cake and the shearing force. Therefore, the filtration speed decreases. Thus, the filtration pressure difference is 2
Making it higher than 0 kg / cm ² only lowers the filtration performance.

The reaction pressure and the slurry side pressure in the filter can be set completely separately by using a circulation pump. But,
For example, if the pressure on the filter side is lower than the reactor pressure,
Not only is there a power loss due to pressure increase, but also because the reactant adsorbed on the catalyst surface repeatedly absorbs and desorbs, the catalyst activity is greatly reduced, and a by-product is easily generated. Therefore, it is desirable that the pressure of the reactor and the pressure of the slurry on the side of the filter be substantially equal to the pressure difference of about the flow pressure loss. In addition, the reaction pressure is 1 kg in order to secure a filtration differential pressure.
It is desirable that the reaction be a pressurization reaction of at least / cm ² gauge pressure.

The temperature of the slurry in the filter may be such that the slurry is kept in a fluid state in a liquid phase. That is, it is only necessary to keep the filter from boiling or solidifying in the filter. Usually, the filter is circulated at the temperature of the product in the reactor. For example, when there is a problem with the material of the sealing material, it is conceivable to prevent corrosion by lowering the filter side temperature below the reaction temperature. Therefore, it is not always necessary to make the reaction temperature equal to the filtration temperature.

In a three-phase gas-liquid-solid reaction system, when a sedimentation separator or a liquid cyclone is used, if gas is mixed into the slurry, the filtration performance is reduced by solids entrained in the air bubbles. Although it is necessary to sufficiently separate the gas, in the cross-flow filter, even if the gas is mixed into the slurry, if the liquid phase is a continuous phase, the bubbles in the flowing slurry will be removed from the slurry due to the momentum balance. Does not affect the filtration performance because it hardly exists near the filter wall surface where the flow rate of the slurry flows slowly through the center of the filter tube where the flow rate of the slurry is low.

The following process is considered as a specific reaction system. However, the present invention is not limited to only these processes. FIG. 1 shows a combination of a stirred tank reactor (1), a cross flow filter (2), and a circulation pump (3). FIG. 2 shows the reactor (1),
Combines a cross-flow filter (2) and a circulation pump (3) to spray and circulate the slurry discharged from the cross-flow filter into the gas phase at the upper part of the reactor to prevent gas-liquid contact and absorption. The reaction is performed well.
In this case, since the mixing of solid and liquid and the absorption of gas in the reactor are performed by the circulating slurry by the circulating pump, the stirrer of the reactor is unnecessary as compared with the case of FIG. This eliminates problems such as a shaft seal of a stirrer, particularly in a high-pressure reaction.

FIG. 3 shows a gas lift type reactor (1),
It is a combination of a cross flow filter (2).
In this case, with the liquid circulation method using the principle of the bubble pump,
The circulating pump is not required in the case of FIG. Thus, the reaction system is close to the push-out flow, so that the reactor is smaller than the complete mixing tank. Further, in the cross-flow filter, there is no problem in filtration performance even if gas is mixed into the slurry due to insufficient gas separation.

1 to 3, the installation direction of the filter may be horizontal or vertical. Also, there are no particular restrictions on the direction of slurry inflow / outflow of the filter, such as the upper or lower part of the filter. Further, the shape of the filter medium may be a circular tube or a flat surface. However, when the filtration pressure is high, a circular tube having a high strength is desirable even with the same thickness. In addition, the slurry is
The slurry may flow outside the tube, but it is preferable to flow the slurry into the tube because the slurry flows smoothly.

[0024]

The present invention will be described in more detail with reference to the following examples, but the present invention is not limited to these examples.

[0025]

Example 1 Production of ethylbenzene by a continuous alkylation reaction using benzene and ethylene as raw materials is shown in FIG.
And under the following reaction conditions. Inside a 4 liter SUS316 electromagnetic stirring type autoclave, a thermometer sheath, a raw material liquid introducing tube, a raw material gas introducing tube, and a heat medium tube for temperature adjustment are attached, and further, a reaction liquid extracting nozzle, a circulating liquid returning nozzle, and a liquid level gauge. Provided as a continuous alkylation reactor.

The reaction solution from the reactor was operated through a slurry circulation pump by operating a valve so that a predetermined circulation amount, that is, a cross flow linear velocity became about 1 to 3 m / s. The slurry was supplied to a cross-flow filter to perform solid-liquid separation, the concentrated slurry liquid was returned to the reactor, and the filtrate was discharged to a filtrate tank. This filter was provided with a filter tube of a ceramic porous body (average pore diameter of 1 to 2 microns), and was equipped with a backwashing device so that a backwashing operation could be performed with gas or liquid.

In the alkylation reaction, first, after pretreatment as a catalyst in a reactor, pulverization is performed, and the average particle diameter is 80 to 1.
500 g of Y-type zeolite and 1600 g of benzene liquid which are sorted to 20 microns are charged, and the indication of the liquid level meter in a stirring state is checked. This liquid level is maintained during operation. Next, benzene was continuously supplied by a high-pressure metering pump so that the liquid level of the reactor became the above indicated value (about 18 kg / hr: K at steady state).
g / hour: hereinafter the same), and the catalyst slurry concentration in the reactor was analyzed while circulating the slurry, and it was about 23% by weight. Thereafter, ethylene was supplied so that the reaction pressure became about 15 kg / cm ² gauge, and the reaction was carried out at a reaction temperature of 190 ° C. The reaction solution was withdrawn by adjusting the pressure of the filtrate tank to be equal to or less than the pressure in the filter (the operating pressure difference between the filter and the filtrate tank, that is, the filtration differential pressure was about 0.1 to 2.
0 kg / cm ² ).

As a result, the alkylation reaction and the separation of the reaction solution and the catalyst were carried out smoothly for 800 hours without back washing. Here, the filtration rate rapidly decreased after the start of the reaction, but stabilized after about 100 hours.
It was 50 to 250 l / m ² / hr (filtrate amount per unit time per unit area of the filter: the same applies hereinafter). In addition, in order to see the effect of the reverse cleaning, it was re-start performs the reverse washing, filtration rate, was almost stabilized at about 100 hours after recovered to almost the initial filtration rate. The filtration rate at this time was equivalent to the stable value before back washing.

[0029]

Example 2 Using iminoisophorone (hereinafter abbreviated as IPCI) represented by the following formula (1) as a raw material, isophoronediamine (hereinafter referred to as the following) represented by the following formula (2) by a continuous hydrogenation reaction: (Abbreviated as IPDA).
Here, IPCI was synthesized by a continuous imination reaction in the absence of a catalyst using cyanoisophorone (hereinafter abbreviated as IPCN) represented by the following formula (3) as a raw material.
Here, the hydrogenation reaction used a gas lift type process as shown in FIG. The reaction conditions for the imination reaction and the hydrogenation reaction are shown below.

[0030]

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[0031]

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[0032]

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The imination reactor was a continuous imination reactor using the same 4-liter apparatus as in Example 1 (however, liquid circulation was not performed). The hydrogenation reactor is a vertical tube with a gas-liquid separator at the top, a thermometer sheath, a raw material liquid introduction pipe,
A source gas introduction pipe was attached, a heating medium trace was performed for temperature adjustment, and a reaction liquid extraction nozzle, a circulating liquid return nozzle, a gas extraction nozzle, and a liquid level gauge were provided, to obtain a continuous hydrogenation reactor.

The reaction solution from the imination reactor was supplied to the hydrogenation reactor with a high-pressure metering pump. The circulation of the reaction solution slurry from the hydrogenation reactor was performed by a gas lift. The supply gas to the reactor is a circulating gas obtained by compressing hydrogen gas and exhaust gas corresponding to the reaction consumption. The circulation flow rate of the slurry is adjusted by the supply gas amount, and the cross flow linear velocity is about 1-3 m / s.
And

The filtration of the hydrogenation catalyst slurry was performed in the same manner as in Example 1. This filter was provided with a SUS316 sintered tubular filter (average pore diameter of about 2 microns), and was equipped with a backwashing device so that a backwashing operation could be performed with gas or liquid. In the imination reaction, first, 2.7 kg of the IPCN raw material mixture (IPCN: methanol = 1: 2 by weight ratio) was charged into the imination reactor, and the indication of the liquid level meter in a stirring state was confirmed. The liquid level is maintained during operation.

Next, the IPCN raw material mixture was continuously supplied to the imination reactor by a metering pump (about 6 kg /
hr), and the reaction pressure of the iminoization reaction is about 9 kg / cm ²
Ammonia was supplied so that the reaction temperature became 80 ° C., and the reaction was carried out at a reaction temperature of 80 ° C. The imination reaction solution was withdrawn so that the liquid level in the imination reactor was at the above indicated value, and supplied to the next hydrogenation reactor.

In the hydrogenation reaction, first, a centrifugal sedimentation type particle size distribution analyzer SA-CP was used as a catalyst in a hydrogenation reactor.
3 (manufactured by Shimadzu Corporation), 63 g of a Raney cobalt catalyst having an average particle diameter of 26.2 microns (minimum particle diameter of about 1 to 3 microns) is charged. Next, the above-mentioned imination reaction solution was supplied, hydrogen gas was further supplied, and the catalyst slurry concentration in the reactor was analyzed while circulating the slurry, to be about 19% by weight. Thereafter, the valve of the hydrogen gas extraction part was adjusted so that the reaction pressure of the hydrogenation reaction became 120 kg / cm ² gauge, and the reaction was carried out at a reaction temperature of 120 ° C. The method of extracting the reaction solution was performed by adjusting the pressure of the filtrate tank to be equal to or less than the pressure inside the filter (the operating pressure difference between the filter and the filtrate tank, that is, the filtration pressure difference was about 0.5 to 3.0).
Kg / cm ² ). As a result, the imination reaction / hydrogenation reaction and the separation of the reaction solution and the catalyst were smoothly performed continuously for 500 hours without back washing. After the stabilization, the filtration rate (stable at about 100 hours) was 100 to 200 l / m ² / hr.

[0038]

EXAMPLE 3 A diol represented by the following formula (5) (hereinafter referred to as DIOL) by a continuous hydrogenation reaction using a diol ester represented by the following formula (4) (hereinafter abbreviated as DBE) as a raw material: ) Was carried out in a process as shown in FIG. 2 under the following reaction conditions.

[0039]

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[0040]

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The reactor was partially modified using the same 4 liter apparatus as in Example 1, ie, the stirrer was removed, and the slurry circulating liquid return nozzle was dispersed in the reactor gas phase to contact the gas phase. A continuous hydrogenation reactor equipped with a spray so as to improve the water content was used. Circulation of the reaction solution slurry from the reactor was performed in the same manner as in Example 1. However, the cross flow linear velocity was 3 to 8 m / s.

The filtration of the hydrogenation catalyst slurry was carried out in the same manner as in Example 1. This filter is equipped with a SUS316 sintered tubular filter (average pore diameter about 0.5 micron),
A backwashing device was installed so that a backwashing operation could be performed with gas or liquid. First, the hydrogenation reaction is carried out in a reactor.
Centrifugal sedimentation type particle size distribution analyzer SA-CP3 as catalyst
(Shimazu Seisakusho Co., Ltd.) measured average particle size 3
850 g of a copper chromium catalyst having a particle size of about 5 μm (minimum particle size of about 1 μm) and 1620 g of a DBE liquid are charged, and the liquid level meter is checked under stirring, and the liquid level is maintained during operation. Next, the DBE was adjusted so that the reactor liquid level was at the indicated value.
The liquid is continuously supplied by a high-pressure metering pump (about 3.
0 Kg / hr), and the catalyst slurry concentration in the reactor was analyzed while circulating the slurry, and it was about 27% by weight.
Thereafter, hydrogen was supplied so that the reaction pressure became 250 kg / cm ² gauge, and the reaction was carried out at a reaction temperature of 250 ° C. The reaction solution was withdrawn by adjusting the pressure of the filtrate tank to be equal to or less than the pressure inside the filter (the operating pressure difference between the filter and the filtrate tank, that is, the filtration pressure difference was about 0.5 to 10.0 kg / c).
m ² ).

As a result, the hydrogenation reaction and the separation of the reaction solution and the catalyst were smoothly performed continuously for 500 hours without back washing. The filtration rate after stabilization (stable in about 20 hours) is 100
２００200 l / m ² / hr.

[0044]

[Embodiment 4] In Embodiments 1 and 3, N ₂ was introduced in the middle of the pipe supplied from the slurry circulation pump to the cross flow filter.
Blow gas (about 10% by volume at system temperature and pressure: N ₂
The test was performed to the limit of the gas supply device), and as a result of observing the effect of gas mixture into the slurry, the catalyst separation performance was hardly affected.

[0045]

According to the present invention, by using a cross-flow filter, a catalyst having a particle size of up to several microns can be used, and a reaction and a catalyst separation with a slurry having a high concentration can be performed. Therefore, the size of the reactor can be reduced, and clogging / scaling in a subsequent process due to catalyst outflow and catalyst loss can be suppressed. Further, the period of the backwashing is increased by suppressing the decrease in the filtration rate over time, thereby realizing a continuous and smooth operation for a long period of time. Further, the size of the catalyst separation device can be reduced compared to a sedimentation separator for a system with a slow sedimentation speed, and the system can be applied to a high-pressure system or a system for handling hazardous substances without any problem because it is a closed system.

Further, when a sedimentation separator or a liquid cyclone is used in a gas-liquid-solid three-phase reaction, if gas is mixed into the slurry, the filtration performance is reduced by solids entrained in bubbles. Although it is necessary to sufficiently separate the gas, the cross-flow filter also has an effect that even if gas is mixed into the slurry, the filtration performance is not reduced.

[Brief description of the drawings]

FIG. 1 is a diagram of a reaction apparatus showing an example of an embodiment according to the present invention. (Slurry circulation system with circulation pump, stirring type reactor)

FIG. 2 is a diagram of a reaction apparatus showing an example of an embodiment according to the present invention. (Slurry circulation system with circulation pump, reactor with circulation liquid spray)

FIG. 3 is a diagram of a reaction apparatus showing an example of an embodiment according to the present invention. (Slurry circulation method by gas lift)

FIG. 4 is a diagram showing an example of a known reaction apparatus.

[Explanation of symbols]

 Reference Signs List 1 reactor 2 cross flow filter 3 slurry circulation pump 4 sedimentation separator

──────────────────────────────────────────────────続 き Continuation of the front page (51) Int.Cl. ⁷ Identification symbol FI C07C 211/36 C07C 211/36 (56) References JP-A-1-148318 (JP, A) JP-A-1-242114 (JP) JP-A-50-37701 (JP, A) JP-B-51-41589 (JP, B1) JP-B-39-5602 (JP, B1) JP-B-39-8503 (JP, B1) (58) Field surveyed (Int. Cl. ⁷ , DB name) B01J 8/18-8/46 C07B 61/00

Claims (1)

(57) [Claims] When a liquid reaction product is obtained by a liquid-liquid or liquid-gas contact reaction in the presence of a particulate solid catalyst, (1) a step of obtaining a liquid reaction product in a suspension fluidized bed; (2) Slurry concentration of 3 weight mainly composed of liquid reaction products
% Or more of a catalyst suspension using a filter medium having an average pore diameter of 0.5 to 10 μm, and a cross flow linear velocity of 0.05 m
Separating the liquid reaction product and the concentrated catalyst suspension by filtration in a cross-flow system at a rate of not less than 3 g / sec. (3) circulating the concentrated catalyst suspension to a suspension fluidized bed A continuous reaction method comprising: