Separating device

By incorporating a stirrer and an inner tube sleeve in the separation device, the problem of catalyst deposition in the products of the cyclohexanone ammoniation reaction without tert-butanol solvent was solved, achieving efficient separation of cyclohexanone oxime and catalyst, and ensuring the stability and efficiency of the separation process.

CN223732693UActive Publication Date: 2025-12-30CHINA PETROLEUM & CHEMICAL CORP +1
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Patent Information

Application Number
CN202520064217.2
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-01-10
Publication Date
2025-12-30
Estimated Expiration
2035-01-10

AI Technical Summary

Technical Problem

In the existing technology, the products of the cyclohexanone amination reaction without tert-butanol solvent are not completely separated from the catalyst, which leads to easy catalyst deposition, unstable separation process, and affects separation efficiency.

Method used

A separation device is employed, comprising a vessel body, a stirrer, an inner tube, and an inner sleeve. The stirrer prevents catalyst deposition, and the combination of the inner tube and the inner sleeve reduces catalyst carrying capacity, thereby achieving effective separation of cyclohexanone oxime and the catalyst.

Benefits of technology

This method achieves efficient separation of cyclohexanone oxime and catalyst, prevents catalyst deposition, ensures the continuity and stability of the separation process, and improves separation efficiency.

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Abstract

The utility model relates to the technical field of chemical equipment, and discloses a separation device. The separation device comprises a kettle body, and a stirrer, an inner extending pipe and an inner sleeve which are arranged in the kettle body, the bottom end of the stirrer is arranged close to the bottom of the kettle body; the inner extending pipe is arranged at the top of the kettle body, the inlet end of the inner extending pipe is positioned outside the kettle body, the outlet end of the inner extending pipe is positioned inside the kettle body, and the outlet end of the inner extending pipe is higher than the bottom end of the stirrer; the inner sleeve is arranged in the inner extending pipe in a sleeved mode, and the outlet end of the inner sleeve is higher than the outlet end of the inner extending pipe. A gas phase balance opening is formed in the side wall of the inner extending pipe and is higher than the outlet end of the inner sleeve. According to the separation device, cyclohexanone-oxime and a catalyst in a cyclohexanone ammoximation reaction product without a reaction solvent can be separated, deposition of the catalyst is prevented, and continuous separation is guaranteed.
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Description

TECHNICAL FIELD

[0001] The utility model relates to the technical field of chemical equipment, specifically relates to a catalyst separation device. BACKGROUND

[0002] Cyclohexanone oxime is mainly used for producing caprolactam, and caprolactam is a key raw material for manufacturing nylon-6. At present, the production of cyclohexanone oxime in industry has basically adopted cyclohexanone ammonio-oximation process. The catalytic ammonio-oximation method is more commonly used in industry, which uses titanium-silicon molecular sieve as catalyst, and in the presence of tert-butyl alcohol solvent, cyclohexanone, ammonia and hydrogen peroxide undergo ammonio-oximation reaction to directly generate cyclohexanone oxime, which has the advantages of simple process, low investment, less waste discharge and environmental friendliness.

[0003] In recent years, a new cyclohexanone ammonio-oximation process without tert-butyl alcohol solvent has become an important research direction. When the cyclohexanone ammonio-oximation reaction is carried out without using tert-butyl alcohol solvent, the problems of separation of reaction products and catalyst and catalyst deposition during the separation process need to be solved.

[0004] Patent application CN114436889A discloses a separation method for reaction products of solvent-free cyclohexanone ammonio-oximation. The method uses cross-flow filtration to separate the reaction material containing cyclohexanone oxime, ammonia, water and catalyst, and separates the clear liquid containing water and oxime; the reaction material after separation of the clear liquid is added with inert alkane solvent for extraction, the aqueous phase after extraction is recycled to the reactor, and the obtained organic phase is an oxime solution. However, since the reaction material is a liquid-liquid-solid three-phase, the problem brought by filtration followed by extraction is that the amount of two liquid phases passing through the filter is in an unstable state during filtration, which easily leads to significant fluctuations in the system.

[0005] Patent application CN116617951A discloses a heterogeneous ammonio-oximation reaction separation method. The method sends the mixture of the extraction agent into the separation tower after the discharge line of the ammonio-oximation reaction kettle. In the separation tower, it is divided into light phase and heavy phase, and the light phase and the heavy phase are sent into the first filter and the second filter respectively to separate the catalyst in the light phase and the water in the heavy phase. The main problems of this method are incomplete separation of the light phase and the heavy phase, easy deposition of the catalyst, etc. UTILITY MODEL CONTENTS

[0006] The utility model aims at overcoming the problems in the prior art, and provides a separation device which can separate cyclohexanone oxime and catalyst in the reaction product of solvent-free cyclohexanone ammonio-oximation reaction, prevent catalyst deposition and ensure continuous separation.

[0007] In order to achieve the above-mentioned purpose, the utility model provides a separation device, wherein the separation device comprises a kettle body and a stirrer, an inner extension pipe and an inner sleeve arranged in the kettle body.

[0008] The bottom end of the stirrer is arranged close to the bottom of the kettle body;

[0009] The inner extension pipe is arranged at the top of the kettle body, the inlet end of the inner extension pipe is located outside the kettle body, the outlet end of the inner extension pipe is located inside the kettle body, and the outlet end of the inner extension pipe is higher than the bottom end of the stirrer;

[0010] The inner sleeve pipe is sleeved inside the inner extension pipe, and the outlet end of the inner sleeve pipe is higher than the outlet end of the inner extension pipe;

[0011] The side wall of the inner extension pipe is provided with a gas phase balance port, and the gas phase balance port is higher than the outlet end of the inner sleeve pipe.

[0012] The separation device provided by the utility model can realize separation of cyclohexanone oxime and catalyst in a reaction solvent-free cyclohexanone oximation reaction product; the stirrer arranged in the kettle body of the separation device prevents the catalyst from depositing at the bottom of the kettle body, ensures continuous separation, and improves separation efficiency; the combination of the inner extension pipe and the inner sleeve pipe reduces the carrying amount of the catalyst in the organic phase containing the cyclohexanone oximation reaction product, and ensures separation effect. BRIEF DESCRIPTION OF DRAWINGS

[0013] Figure 1 is a schematic view of the separation device of the utility model embodiment 1;

[0014] Figure 2 is a schematic view of the separation device of the utility model embodiment 2;

[0015] Figure 3 is a schematic view of the separation device of the utility model comparative example 1.

[0016] MARKS DESCRIPTION

[0017] Figure 1 and Figure 2 in,

[0018] 1-kettle body; 2-stirrer;

[0019] 3-inner extension pipe; 4-anti-collision baffle;

[0020] 5-inner sleeve pipe; 6-overflow weir;

[0021] 7-first outlet; 8-second outlet;

[0022] 9-third outlet; 10-gas phase balance port;

[0023] 11-membrane assembly; 12-manifold;

[0024] 13-fourth outlet.

[0025] Figure 3 In some embodiments,

[0026] 1 - kettle body; 2 - inner extension pipe;

[0027] 3 - anti-collision baffle; 4 - overflow weir;

[0028] 5 - first outlet; 6 - second outlet;

[0029] 7 - third outlet. DETAILED DESCRIPTION

[0030] The endpoints of the ranges and any values disclosed herein are not limited to the precise values recited as the exact dimensions are not critical to the characteristics of the invention. The disclosed ranges are therefore to be understood to include values approximating these ranges. In terms of numeric ranges, the endpoints of each range, the endpoints of each range and individual point values, and individual point values can be combined with one another to generate one or more new numeric ranges, which should be considered as being specifically disclosed herein.

[0031] The utility model provides a kind of separation device, wherein the separation device includes kettle body 1 and is set in the agitator 2 of kettle body 1, inner extension pipe 3 and inner sleeve pipe 5;

[0032] The bottom end of the agitator 2 is arranged close to the bottom of the kettle body 1.

[0033] The inner extension pipe 3 is arranged at the top of the kettle body 1, the inlet end of the inner extension pipe 3 is located outside the kettle body 1, the outlet end of the inner extension pipe 3 is located inside the kettle body 1, and the outlet end of the inner extension pipe 3 is higher than the bottom end of the agitator 2.

[0034] The inner sleeve pipe 5 is sleeved inside the inner extension pipe 3, and the outlet end of the inner sleeve pipe 5 is higher than the outlet end of the inner extension pipe 3.

[0035] A gas phase balance port 10 is formed on the side wall of the inner extension pipe 3, and the gas phase balance port 10 is higher than the outlet end of the inner sleeve pipe 5.

[0036] The separation device provided by the utility model can realize the separation of cyclohexanone oxime and catalyst in the cyclohexanone oxime reaction product without reaction solvent, the agitator is arranged in the kettle body of the separation device to prevent the catalyst from depositing at the bottom of the kettle body, ensure the continuous separation, and improve the separation efficiency; the combination of the inner extension pipe and the inner sleeve pipe reduces the carrying amount of catalyst in the organic phase containing the cyclohexanone oxime reaction product, and ensures the separation effect.

[0037] In the utility model, preferably, the inlet end of the inner sleeve pipe 5 is flush with the inlet end of the inner extension pipe 3, and the annular space region formed by the inlet end of the inner sleeve pipe 5 and the inlet end of the inner extension pipe 3 is closed.

[0038] Preferably, the ratio of the length of the inner sleeve 5 to the length of the inner extension pipe 3 is 5-30:1, preferably 8-25:1. By optimizing the length of the inner extension pipe and the inner sleeve, the loss of organic phase product catalyst entrainment can be reduced. When the length ratio of the two is not within the above range, the loss of organic phase product catalyst entrainment increases, resulting in waste of catalyst and poor separation effect of organic phase product.

[0039] Preferably, the ratio of the length of the inner extension pipe 3 extending below the upper tangent of the kettle body 1 to the vertical distance between the upper tangent and the lower tangent of the kettle body 1 is 0.3-0.95:1, preferably 0.4-0.9:1. By controlling the position of the inner extension pipe in the kettle body, the catalyst organic phase entrainment is further inhibited, avoiding waste of catalyst and improving the separation effect.

[0040] In the utility model, it needs to be explained that the upper tangent of the kettle body refers to the tangential section of the intersection between the upper head and the cylinder wall of the kettle body; the lower tangent of the kettle body refers to the tangential section of the intersection between the lower head and the cylinder wall of the kettle body.

[0041] In the utility model, the length of the inner extension pipe above the upper tangent of the kettle body is not particularly limited, as long as the length of the inner extension pipe extending below the upper tangent of the kettle body is met.

[0042] In the utility model, preferably, the bottom end of the stirrer 2 is provided with a stirring paddle.

[0043] In the utility model, the type of the stirring paddle is not particularly limited. Preferably, the stirring paddle is selected from at least one of a propeller stirring paddle, a turbine stirring paddle, an anchor stirring paddle and a frame stirring paddle.

[0044] In the utility model, preferably, the number of layers of the stirring paddle is 1-3 layers.

[0045] In the utility model, preferably, the kettle body 1 is further provided with a anti-collision baffle 4, and the anti-collision baffle 4 is arranged close to the outlet end of the inner extension pipe 3. By setting the anti-collision baffle, the material to be treated containing the catalyst is effectively buffered, preventing liquid impact from causing the interface of the organic phase and the aqueous phase to fluctuate.

[0046] In the utility model, preferably, an overflow weir 6 is arranged on the inner wall of the kettle body 1, and the overflow weir 6 is arranged close to the upper part of the kettle body 1.

[0047] In the utility model, the shape of the overflow weir is not particularly limited, and under the preferred condition, the overflow weir 6 is an L-shaped plate, and one end of the L-shaped plate is connected with the inner wall of the kettle body 1.

[0048] The utility model discloses, preferably, a first outlet 7 is arranged on the kettle body 1, and the first outlet 7 is communicated with the overflow weir 6.

[0049] The utility model discloses, preferably, a second outlet 8 is arranged at the bottom of the kettle body 1, and the second outlet 8 is communicated with the space at the bottom of the kettle body 1.

[0050] The utility model discloses, preferably, a third outlet 9 is arranged at the top of the kettle body 1, and the third outlet 9 is communicated with the space at the top of the kettle body 1.

[0051] The utility model discloses, preferably, the shape of the lower head of the kettle body 1 is at least one of oval, spherical and conical, preferably conical.

[0052] The utility model discloses, preferably, a membrane assembly 11 and a collecting pipe 12 are optionally arranged in the kettle body 1, one end of the membrane assembly 11 is closed, and the other end of the membrane assembly 11 is communicated with the collecting pipe 12.

[0053] The utility model discloses, preferably, the membrane assembly 11 includes one or more membrane tubes.

[0054] The utility model discloses, preferably, the setting mode of the plurality of membrane tubes is not particularly limited, which can be series setting or parallel setting, preferably parallel setting.

[0055] The utility model will be described in detail through the following examples. In the following examples, if no special description is made, the raw materials used are commercially available.

[0056] Example 1

[0057] As Figure 1As shown, the separation device comprises a kettle body 1, and a stirrer 2, an inner extension pipe 3 and an inner sleeve 5 arranged in the kettle body 1; the bottom end of the stirrer 2 is arranged close to the bottom of the kettle body 1, and the bottom end of the stirrer 2 is provided with a stirring paddle (specifically a turbine paddle), and the number of layers of the stirring paddle is 1; the inlet end of the inner extension pipe 3 is located outside the kettle body 1, the outlet end of the inner extension pipe 3 is located inside the kettle body 1, the outlet end of the inner extension pipe 3 is higher than the bottom end of the stirrer 2, the ratio of the length of the inner extension pipe 3 extending into the kettle body 1 below the tangent line to the vertical distance between the tangent line and the tangent line of the kettle body 1 is 0.85:1; the outlet end of the inner extension pipe 3 is provided with a anti-collision baffle 4, and the kettle body 1 is further provided with an overflow weir 6 (the overflow weir 6 is an L-shaped plate, one end of the L-shaped plate is connected with the inner wall of the kettle body 1) and a first outlet 7 communicating with the overflow weir 6; the kettle body 1 is provided with a second outlet 8 at the bottom and a third outlet 9 at the top; the inner sleeve 5 is sleeved in the inner extension pipe 3, the outlet end of the inner sleeve 5 is higher than the outlet end of the inner extension pipe 3, the inlet end of the inner sleeve 5 is flush with the inlet end of the inner extension pipe 3, the annular space area formed by the inlet end of the inner sleeve 5 and the inlet end of the inner extension pipe 3 is closed, and the length ratio of the inner extension pipe 3 to the inner sleeve 5 is 15:1; the side wall of the inner extension pipe 3 is provided with a gas phase balance port 10, which communicates with the space at the top of the kettle body 1 to ensure gas phase balance.

[0058] As shown in the catalyst separation device, Figure 1 The mixture of cyclohexanone aminooxidation reaction product and toluene (cyclohexanone aminooxidation reaction product and toluene are mixed, cyclohexanone oxime in the cyclohexanone aminooxidation reaction product is extracted into the toluene phase to obtain a mixture of cyclohexanone aminooxidation reaction product and toluene, wherein the content of cyclohexanone oxime is 5 mass%, toluene is 10 mass%, ammonia is 5 mass%, catalyst is 3.2 mass%, and water is 76.8 mass%) is subjected to two-phase separation, specifically:

[0059] The mixture of cyclohexanone aminooxidation reaction product and toluene is transported into the inner extension pipe 3 through the inner sleeve 5, and then transported into the kettle body 1 through the inner extension pipe 3 and the anti-collision baffle 4, the operating pressure (separation pressure) of the kettle body 1 is 0.3 MPaG, and the mixture of cyclohexanone aminooxidation reaction product and toluene is subjected to two-phase separation in the kettle body 1 to obtain an organic phase containing cyclohexanone oxime and toluene, and an aqueous phase containing catalyst, ammonia and water, the organic phase is transported outside the kettle body 1 from the first outlet 7 through the overflow weir 6, and the aqueous phase is transported outside the kettle body 1 through the second outlet 8 under the action of the stirring paddle (the rotating speed is 180 rpm) of the stirrer 2.

[0060] After the device is stably operated for 48 hours, the organic phase is taken from the first outlet 7, the amount of catalyst loss is determined by measuring the turbidity of the organic phase; the water phase is taken from the second outlet 8, the volume ratio of the organic phase in the water phase is measured after the water phase is left for 30 minutes, the oil-carrying condition of the water phase is determined; the mass content of the catalyst in the water phase is measured to determine whether the catalyst is accumulated in the separation device. The test results are shown in Table 1.

[0061] Example 2

[0062] As shown in Figure 2 , the separation device comprises a kettle body 1 and a stirrer 2, an inner extension pipe 3 and an inner sleeve 5 arranged in the kettle body 1; the bottom end of the stirrer 2 is arranged close to the bottom of the kettle body 1, the bottom end of the stirrer 2 is provided with a stirring paddle (specific type is a turbine paddle), the number of layers of the stirring paddle is 1 layer; the inlet end of the inner extension pipe 3 is located outside the kettle body 1, the outlet end of the inner extension pipe 3 is located inside the kettle body 1, the outlet end of the inner extension pipe 3 is higher than the bottom end of the stirrer 2, the ratio of the length of the inner extension pipe 3 extending into the kettle body 1 below the upper tangent line to the vertical distance between the upper tangent line and the lower tangent line of the kettle body 1 is 0.85:1; the outlet end of the inner extension pipe 3 is provided with a anti-impact baffle 4, the kettle body 1 is further provided with an overflow weir 6 (the overflow weir 6 is an L-shaped plate, one end of the L-shaped plate is connected with the inner wall of the kettle body 1) and a first outlet 7 communicating with the overflow weir 6; the kettle body 1 is provided with a second outlet 8 at the bottom and a third outlet 9 at the top; the inner sleeve 5 is sleeved in the inner extension pipe 3, the outlet end of the inner sleeve 5 is higher than the outlet end of the inner extension pipe 3, the inlet end of the inner sleeve 5 is flush with the inlet end of the inner extension pipe 3, the annular space region formed by the inlet end of the inner sleeve 5 and the inlet end of the inner extension pipe 3 is closed, the length ratio of the inner extension pipe 3 to the inner sleeve 5 is 15:1; a gas phase balance port 10 is formed on the side wall of the inner extension pipe 3, the gas phase balance port 10 communicates with the space at the top of the kettle body 1 to ensure the gas phase balance.

[0063] A membrane assembly 11 (the membrane assembly 11 comprises 24 parallel membrane tubes) is arranged below the anti-impact baffle 4, one end of the membrane tube is closed, the other end is connected with a manifold 12, the manifold 12 is connected with a fourth outlet 13, the liquid in the water phase penetrates from the outer surface of the membrane tube to the inner side of the membrane tube and obtains a clear liquid, the clear liquids in different membrane tubes are collected through the manifold 12 and then discharged, a backwashing pipeline is arranged on the clear liquid discharge pipeline, and the washing liquid is filtered clear liquid; the material of the membrane tube is 316 stainless steel, and the filtration precision is 0.2 μm.

[0064] In the same way as Figure 2As shown in the catalyst separation device, the mixture of the cyclohexanone aminooxidation reaction product and toluene (the cyclohexanone aminooxidation reaction product and toluene are mixed, the cyclohexanone oxime in the cyclohexanone aminooxidation reaction product is extracted into the toluene phase, and the mixture of the cyclohexanone aminooxidation reaction product and toluene is obtained, wherein the content of the cyclohexanone oxime is 5% by mass, the content of the toluene is 10% by mass, the content of the ammonia is 5% by mass, the content of the catalyst is 3.2% by mass, and the content of the water is 76.8% by mass) is subjected to two-phase separation, and specifically:

[0065] The mixture of the cyclohexanone aminooxidation reaction product and toluene is transported into the inner extension pipe 3 through the inner sleeve pipe 5, and then transported into the kettle body 1 through the inner extension pipe 3 and the anti-impact baffle 4. The operating pressure (separation pressure) of the kettle body 1 is 0.3 MPaG. The mixture of the cyclohexanone aminooxidation reaction product and toluene is subjected to two-phase separation in the kettle body 1 to obtain an organic phase containing cyclohexanone oxime and toluene and an aqueous phase containing a catalyst, ammonia and water. The organic phase is transported outside the kettle body 1 from the first outlet 7 through the overflow weir 6. The liquid in the aqueous phase penetrates from the outer surface of the membrane tube to the inner side of the membrane tube to obtain a clear liquid which is discharged through the collecting pipe 12 and the fourth outlet 13. The filtered aqueous phase is transported outside the kettle body 1 through the second outlet 8 under the action of the stirring paddle (the rotating speed is 180 rpm) of the stirrer 2.

[0066] The turbidity of the organic phase, the volume ratio of the organic phase in the aqueous phase and the mass content of the catalyst in the aqueous phase are measured according to the method of Example 1, and the test results are shown in Table 1.

[0067] Comparative Example 1

[0068] As shown in the catalyst separation device, the mixture of the cyclohexanone aminooxidation reaction product and toluene (the cyclohexanone aminooxidation reaction product and toluene are mixed, the cyclohexanone oxime in the cyclohexanone aminooxidation reaction product is extracted into the toluene phase, and the mixture of the cyclohexanone aminooxidation reaction product and toluene is obtained, wherein the content of the cyclohexanone oxime is 5% by mass, the content of the toluene is 10% by mass, the content of the ammonia is 5% by mass, the content of the catalyst is 3.2% by mass, and the content of the water is 76.8% by mass) is subjected to two-phase separation, and specifically: Figure 3 As shown in the catalyst separation device, the mixture of the cyclohexanone aminooxidation reaction product and toluene (the cyclohexanone aminooxidation reaction product and toluene are mixed, the cyclohexanone oxime in the cyclohexanone aminooxidation reaction product is extracted into the toluene phase, and the mixture of the cyclohexanone aminooxidation reaction product and toluene is obtained, wherein the content of the cyclohexanone oxime is 5% by mass, the content of the toluene is 10% by mass, the content of the ammonia is 5% by mass, the content of the catalyst is 3.2% by mass, and the content of the water is 76.8% by mass) is subjected to two-phase separation, and specifically:

[0069] Figure 3 As shown in the catalyst separation device, the mixture of the cyclohexanone aminooxidation reaction product and toluene (the cyclohexanone aminooxidation reaction product and toluene are mixed, the cyclohexanone oxime in the cyclohexanone aminooxidation reaction product is extracted into the toluene phase, and the mixture of the cyclohexanone aminooxidation reaction product and toluene is obtained, wherein the content of the cyclohexanone oxime is 5% by mass, the content of the toluene is 10% by mass, the content of the ammonia is 5% by mass, the content of the catalyst is 3.2% by mass, and the content of the water is 76.8% by mass) is subjected to two-phase separation, and specifically: ​

[0070] The mixture of the cyclohexanone ammoxyl reaction product and toluene is transported into the kettle body 1 through the inner extension pipe 2 and the anti-collision baffle 3, the operating pressure (separation pressure) of the kettle body 1 is 0.3 MPaG, the mixture of the cyclohexanone ammoxyl reaction product and toluene is subjected to two-phase separation in the kettle body 1, and an organic phase containing cyclohexanone oxime and toluene and an aqueous phase containing catalyst, ammonia and water are obtained, the organic phase is transported out of the kettle body 1 from the first outlet 5 through the overflow weir 4, and the aqueous phase is transported out of the kettle body 1 through the second outlet 6.

[0071] The turbidity of the organic phase, the volume ratio of the organic phase in the aqueous phase and the mass content of the catalyst in the aqueous phase are measured according to the method of Example 1, and the test results are shown in Table 1.

[0072] Table 1

[0073] Item Example 1 Example 2 Comparative Example 1 Organic phase turbidity, pg / g 2 2 18 Volume content of organic phase in aqueous phase, % 0.1 0.5 0.1 Mass content of catalyst in aqueous phase, % 3.68 3.65 3.25

[0074] Note: The theoretical value of the mass content of the catalyst in the aqueous phase is 3.7%.

[0075] It can be seen from the results of the examples and the comparative examples that, compared with the comparative examples, the separation device provided by the present application can realize the separation of the organic phase containing the cyclohexanone ammoxyl reaction product and the catalyst, and the separation effect is better.

[0076] The preferred embodiments of the present application are described in detail above, but the present application is not limited thereto. Within the technical concept of the present application, various simple modifications can be made to the technical solutions of the present application, including the combination of various technical features in any other suitable manner, and these simple modifications and combinations should also be considered as the disclosed content of the present application, and all fall within the protection scope of the present application.

Claims

1. A separating device, characterized in that The separation device comprises a kettle body (1) and a stirrer (2), an inner extension pipe (3) and an inner sleeve pipe (5) arranged in the kettle body (1); The bottom end of the stirrer (2) is arranged close to the bottom of the kettle body (1); The inner extension pipe (3) is arranged at the top of the kettle body (1), the inlet end of the inner extension pipe (3) is located outside the kettle body (1), the outlet end of the inner extension pipe (3) is located inside the kettle body (1), and the outlet end of the inner extension pipe (3) is higher than the bottom end of the stirrer (2); The inner sleeve pipe (5) is arranged inside the inner extension pipe (3), and the outlet end of the inner sleeve pipe (5) is higher than the outlet end of the inner extension pipe (3); The side wall of the inner extension pipe (3) is provided with a gas phase balance port (10), and the gas phase balance port (10) is higher than the outlet end of the inner sleeve pipe (5).

2. The separation device of claim 1, wherein, The inlet end of the inner sleeve pipe (5) is flush with the inlet end of the inner extension pipe (3), and the annular space region formed by the inlet end of the inner sleeve pipe (5) and the inlet end of the inner extension pipe (3) is closed.

3. The separation device of claim 1 or 2, wherein, The length ratio of the inner sleeve pipe (5) to the inner extension pipe (3) is 5-30:

1.

4. The separation device of claim 1 or 2, wherein, The ratio of the length of the inner extension pipe (3) extending into the kettle body (1) below the tangent line to the vertical distance between the tangent line and the lower tangent line of the kettle body (1) is 0.3-0.95:

1.

5. The separation device of claim 1 or 2, wherein, The bottom end of the stirrer (2) is provided with a stirring paddle, and the stirring paddle is selected from at least one of a propeller stirring paddle, a turbine stirring paddle, an anchor stirring paddle and a frame stirring paddle.

6. The separation device of claim 1 or 2, wherein, The kettle body (1) is further provided with a anti-impact baffle (4) arranged close to the outlet end of the inner extension pipe (3).

7. The separation device of claim 1 or 2, wherein, An overflow weir (6) is arranged on the inner wall of the kettle body (1), and the overflow weir (6) is arranged close to the upper part of the kettle body (1).

8. The separation device of claim 7, wherein, A first outlet (7) is arranged on the kettle body (1), and the first outlet (7) is in communication with the overflow weir (6).

9. The separation device of claim 1 or 2, wherein, A second outlet (8) is arranged at the bottom of the kettle body (1), and the second outlet (8) is in communication with the space at the bottom of the kettle body (1).

10. The separation device of claim 1 or 2, wherein, A third outlet (9) is arranged at the top of the kettle body (1), and the third outlet (9) is in communication with the space at the top of the kettle body (1).

11. The separation device of claim 1 or 2, wherein, The kettle body (1) is further optionally provided with a membrane assembly (11) and a collecting pipe (12), one end of the membrane assembly (11) is closed, and the other end of the membrane assembly (11) is in communication with the collecting pipe (12).

Citation Information

Patent Citations

  • Heterogeneous ammoximation reaction separation device and method

    CN116617951A