Method and system for treating production materials from organic chemical process

By combining processes such as standstill, distillation and filtration, the organic chemical process production materials are processed, and the problems of low catalyst recovery and complex organic phase treatment process are solved, efficient and environmentally friendly material separation and recycling are achieved, and production efficiency and economicality are improved.

CN120114869APending Publication Date: 2025-06-10ZHEJIANG BALING HENGYI CAPROLACTAM
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Patent Information

Application Number
CN202510433895.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-08
Publication Date
2025-06-10

AI Technical Summary

Technical Problem

In the prior art, when processing organic chemical process production materials, the catalyst recovery rate is low, the separation efficiency is low, and the organic phase treatment process is complex and the energy consumption is high, resulting in resource consumption and environmental pollution problems.

Method used

The organic phase and catalyst phase in the production material are separated by a combination of standstill method, distillation method, filtration method or settlement evaporation method. The material is fully separated by adding an aqueous extract, which improves the separation efficiency, and recovers the solid catalyst by reverse rinsing.

Benefits of technology

It realizes efficient, rapid and environmentally friendly separation and recovery of catalysts and organic materials, reduces raw material consumption and resource waste, and improves production efficiency and economicality.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a method and a system for treating production materials from an organic chemical process. The production materials comprise an initial catalyst phase and an organic phase. The method comprises the following steps: feeding a production material into a first separation device, adding a water-based extraction liquid, and carrying out phase separation to obtain an organic phase, a water phase and a solid catalyst phase; a first part of organic phase obtained through separation is discharged to a material receiving device; performing first heating evaporation on the first residual material comprising the second part of organic phase, the water phase and the solid catalyst phase, so that a first gas phase mixture comprising all the second part of organic phase, part of water phase and unreacted raw material gas is separated from the top of the first separation device; and discharging a second residual material comprising the residual water phase and the solid catalyst phase from the bottom of the first separation device, and carrying out filter pressing or sedimentation evaporation to obtain the solid catalyst and the water phase. The method for separating the catalyst and the organic material is simple in process, low in energy consumption, high in separation recovery rate and good in economic and environmental benefits.
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Description

Technical Field

[0001] The present invention relates to the technical field of organic chemical engineering, and in particular, to a method and system for treating production materials from an organic chemical process. Background Art

[0002] In the organic chemical process, some solid catalysts are crucial for maintaining the continuous stability and production efficiency of industrial processes due to their high activity, high selectivity, and relatively high stability in reducing and oxidizing atmospheres. During the operation of the reaction system, for various reasons, such as when the catalyst is deactivated, the catalyst is recovered, the reaction conditions and reaction selectivity are controlled, the product is separated, and environmental protection requirements and equipment maintenance are considered, the catalyst needs to be withdrawn from the system and the material production needs to be reorganized. Therefore, a suitable method is required to separate it from the production materials. At the same time, the withdrawn materials may also contain various organic substances and other hazardous chemical wastes that need to be treated and recycled.

[0003] The liquid-phase benzene hydrogenation reaction is currently the best way for large-scale industrial production of cyclohexane. In a liquid medium, benzene and hydrogen undergo an addition reaction. By optimizing the reaction conditions and catalysts, the reaction selectivity and efficiency can be improved, and the generation of by-products can be reduced, thereby achieving a more economical and environmentally friendly production process in industry.

[0004] CN 102161008B discloses a method for recovering a catalyst for the partial hydrogenation of benzene to prepare cyclohexane. The reaction product obtained from the benzene partial hydrogenation reaction system is sent to a settler to separate the organic phase containing organic materials and the aqueous phase. The aqueous phase is returned to the benzene partial hydrogenation reaction system, and the separated organic phase enters a filter to separate solid substances such as the catalyst. The filter cake is returned to the benzene partial hydrogenation reaction system. Further, the residual gas phase is separated from the organic phase filtrate by flash evaporation, and residual gases such as unreacted hydrogen are removed. The organic phase after flash evaporation is washed with water, and the raffinate organic phase is further separated by rectification. This method has incomplete separation of the aqueous phase, organic phase, and catalyst by simple sedimentation separation. The aqueous phase still contains residual organic substances and catalysts, resulting in low catalyst recovery rate and separation efficiency. Moreover, the solid catalyst filter cake separated from the organic phase adsorbs organic substances on its surface, with low cleanliness, and is not suitable for direct recovery or return to the production system, making it difficult to achieve catalyst regeneration. At the same time, the organic phase needs to undergo complex processes such as sedimentation, filtration, extraction, and rectification, with high energy consumption and low recovery rate. The untreated residual organic phase and catalyst in the aqueous phase may also cause environmental pollution if discarded.

[0005] Therefore, a reasonable method for treating the production materials of the organic chemical process is needed to improve the recovery efficiency of the catalyst and organic raw materials in the production materials, reduce resource consumption and environmental pollution, and improve the economy and production efficiency of the production system. Summary of the Invention

[0006] In view of this, in a first aspect, the present invention provides a method for processing production materials from an organic chemical process, the production materials including an initial catalyst phase and an organic phase, comprising the following steps:

[0007] (1) Feeding the production materials into a first separation device, adding an aqueous extraction liquid, stirring and mixing, and then standing for phase separation. After standing, the production materials are stratified from top to bottom into an organic phase, an aqueous phase, and a solid catalyst phase;

[0008] (2) Discharging a first part of the upper organic phase from the first separation device to a material receiving device;

[0009] (3) In the first separation device, performing first heating evaporation on a first remaining material including a second part of the organic phase, the aqueous phase, and the solid catalyst phase, so as to separate a first gas-phase mixture from the top of the first separation device, the first gas-phase mixture including all of the second part of the organic phase, a part of the aqueous phase, and unreacted raw material gas;

[0010] (4) Discharging a second remaining material including the remaining aqueous phase and the solid catalyst phase from the bottom of the first separation device, subjecting the second remaining material to pressure filtration to separate a solid catalyst and an aqueous phase; or after the second remaining material is allowed to settle and phase-separate, forming an aqueous phase and a solid catalyst phase, discharging the aqueous phase, and performing second heating evaporation on the solid catalyst phase to obtain a solid catalyst and a second gas-phase mixture.

[0011] Further, in step (2), the separated first part of the upper organic phase is subjected to solid-liquid separation and reverse flushing, the organic matter is discharged from the first separation device to the material receiving device, and the solid catalyst entrained in the first part of the organic phase is recovered into the first separation device.

[0012] Preferably, the weight ratio of the production materials to the aqueous extraction liquid is (1-3):1.

[0013] Further, the first gas-phase mixture and the second gas-phase mixture respectively enter the material receiving device after condensation.

[0014] Further, the materials entering the material receiving device are suctioned to discharge the gas-phase part therein, and the remaining liquid-phase part is allowed to stand and layer-separated, and the organic phase and the aqueous phase are respectively discharged.

[0015] Further, the temperature of the first heating evaporation is 60-82°C, the temperature of the second heating evaporation is 90-100°C; the pressure of the pressure filtration is 0.5-1.0 MPa.

[0016] Further, the organic chemical process is a liquid-phase benzene hydrogenation process.

[0017] Further, the aqueous extraction liquid is water, the organic phase is benzene, the raw material gas is hydrogen, the catalyst is a deactivated catalyst, and the backwashing is performed by water rinsing.

[0018] On the other hand, the present invention also provides a system for treating production materials from an organic chemical process, the production materials including an initial catalyst phase and an organic phase, and the system sequentially including, in the flow direction of the production materials:

[0019] A first separation device, equipped with a stirring device and a first heating component, and used for receiving production materials and an aqueous extraction liquid;

[0020] A material receiving device, communicating with the first separation device, and receiving the organic phase, a part of the aqueous phase, and unreacted raw material gas from the first separation device;

[0021] A second separation device, communicating with the bottom of the first separation device, and used for separating the remaining aqueous phase and the solid catalyst phase.

[0022] Further, the material receiving device communicates with the middle side wall of the first separation device and is used for receiving the organic phase discharged from the first separation device.

[0023] A solid-liquid separation device is provided between the material receiving device and the middle side wall of the first separation device, and is used for intercepting the solid catalyst entrained in the discharged organic phase; and a backwashing pipe is used for flushing the intercepted solid catalyst back into the first separation device.

[0024] Further, the material receiving device communicates with the top of the first separation device and is used for receiving a first gas-phase mixture including all the remaining organic phase, a part of the aqueous phase, and unreacted raw material gas.

[0025] Further, the system for treating production materials from an organic chemical process further includes a cooling device provided between the material receiving device and the top of the first separation device, and is used for condensing the materials entering therein.

[0026] Further, the system further includes a catalyst storage device and a first aqueous phase storage device communicating with the bottom of the second separation device.

[0027] Further, the second separation device is a pressure filtration device and / or a sedimentation evaporation device.

[0028] Further, the system further includes a vacuum generating device communicating with the top of the material receiving device, and an organic phase storage device and a second aqueous phase storage device communicating with the bottom of the material receiving device.

[0029] Further, the solid-liquid separation device is a filter screen or a filter.

[0030] The method for processing production materials from organic chemical processes disclosed in the present invention adopts a process combining the static settling method, the distillation method, the filtration method or the sedimentation evaporation method to separate the organic materials and the solid catalyst phase, and provides a system for processing production materials from organic chemical processes. It can efficiently, quickly and environmentally separate and recover the catalyst and organic materials, reduce the consumption of raw materials and waste of resources, improve production efficiency and reduce economic costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 FIG. is a schematic diagram of a system for processing production materials from organic chemical processes according to the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0032] The present invention will be further described in detail below with reference to the accompanying drawings, but is not limited to the following embodiments. Those skilled in the same field can propose other embodiments within the technical solution framework of the present invention, but these embodiments are all included within the protection scope of the present invention.

[0033] The present invention adopts a process combining the static settling method, the distillation method, the filtration method or the sedimentation evaporation method to separate the organic phase and the initial catalyst phase in the production materials from organic chemical processes. By adding an aqueous extraction liquid, the production materials are fully phase-separated, improving the separation efficiency of the production materials. At the same time, the backwashing of the solid catalyst is increased, improving the raw material recovery rate. It can efficiently and quickly separate and process the catalyst and organic materials, reducing energy consumption and raw material waste.

[0034] According to one embodiment, the present invention provides a method for processing production materials from organic chemical processes, and the production materials include an initial catalyst phase and an organic phase.

[0035] In the method of the present invention, first, the production materials generated by the organic chemical process are fed into a first separation device, and an aqueous extraction liquid is added to the first separation device. After stirring and mixing, it is left to stand, so that the production materials are stratified from top to bottom into an organic phase, an aqueous phase and a solid catalyst phase.

[0036] Static separation is a commonly used material separation method in industrial production, which separates by using the density difference between different materials. The separation effect of the traditional static separation method is greatly affected by the density difference. When separating the organic phase and the catalyst by static separation, in a chemical process system with oil-water emulsification or fine catalyst particles, due to the small density difference between the two phases, the separation effect is not good. The method of the present invention adds an aqueous extraction liquid in the first stage of material separation, increasing the density difference between the phases, and can improve the separation effect of the organic materials and the catalyst.

[0037] Specifically, the above-mentioned organic chemical process can be a liquid-phase benzene hydrogenation process. The liquid-phase benzene hydrogenation reaction is currently the best way to industrially produce the chemical raw material cyclohexane on a large scale. In a liquid medium, benzene and hydrogen undergo an addition reaction. Separating and recovering the organic phase and the catalyst in the production materials generated by the liquid-phase benzene hydrogenation process is an important step in the liquid-phase benzene hydrogenation process, which can improve the separation efficiency of the production materials, thereby realizing a more economical and environmentally friendly production process in industry.

[0038] In the production materials from the liquid-phase benzene hydrogenation process treated by the method of the present invention, the organic phase can include cyclohexane, benzene, and unreacted hydrogen gas. The initial catalyst phase can include an aqueous suspension of the catalyst, where the catalyst can be, for example, a ruthenium catalyst, a platinum catalyst, or a zinc catalyst. Further, the initial catalyst phase can also include zirconia as a dispersant as needed. Conventional separation methods are difficult to fully separate the catalyst phase into solid catalyst and water, especially after evaporation treatment in the separation device, it is easy to deposit on the wall of the separation device to form catalyst scale.

[0039] In the method of the present invention, after the production materials are fed into the first separation device, an aqueous extraction liquid is first added to promote the more complete phase separation of the organic phase and the initial catalyst phase in the production materials into three phases: an organic phase, an aqueous phase, and a catalyst phase. Further, the weight ratio of the production materials to be treated to the aqueous extraction liquid can be (1 - 3):1, for example, 2:1. Preferably, the aqueous extraction liquid can be water, such as deionized water. Using water as the intermediate phase between the organic phase and the solid catalyst phase, the polarity and density difference between water and the other two phases are large, which can improve the separation effect, and the generated aqueous phase is easy to treat, thereby simplifying the separation and recovery process. Within the proportion range of the present invention, a good phase separation effect can be achieved. If the amount of the added aqueous extraction liquid is too low, the three-phase stratification of the production materials cannot be achieved. If the amount of the added aqueous extraction liquid is too large, the evaporation treatment amount and heating energy consumption in the separation device will be too large.

[0040] Further, the upper-layer organic phase after stratification is discharged from the first separation device to a material receiving device. In one embodiment, it can be discharged by an overflow method, for example, discharged from the middle side wall of the first separation device. By separating the organic phase in this way, the purity of the organic phase can be improved, and the loss of the organic phase in complex operations can be avoided.

[0041] In the above step, when the upper-layer organic phase is discharged from the first separation device to the material receiving device, a part of the organic phase remains in the first separation device. The organic phase discharged to the material receiving device is called the first part of the organic phase, and the organic phase remaining in the first separation device is called the second part of the organic phase.

[0042] According to an embodiment of the method of the present invention, during the process of discharging the first part of the organic phase from the first separation device to the material receiving device, solid-liquid separation is performed to separate the solid catalyst entrained in the first part of the organic phase, so as to ensure that the substances in the material receiving device are only organic substances and aqueous extraction liquid. This solid-liquid separation process can be carried out by setting a filter screen or a filter. Further, the pore size of the filter screen or the filter can be 140 to 160 microns, for example, it can be 150 microns.

[0043] Preferably, after the entrained solid catalyst is intercepted from the first part of the organic phase by the filter membrane, backwashing can be carried out to wash the intercepted solid catalyst back into the first separation device. This backwashing process can prevent the filter screen or the filter from being blocked by the solid catalyst and keep the pipeline unobstructed. Further, after this backwashing process, the first treatment device usually needs to be left standing for more than 2 hours again, so that the solid catalyst phase precipitates and stratifies again, and then the discharging operation is carried out. Therefore, the phase separation effect can be further improved, the impurities in the organic phase can be reduced, the material phase composition in the material receiving device can be made simpler, it is easy to separate the non-solid phase subsequently, and at the same time, the catalyst recovery rate can be improved.

[0044] In the method of the present invention, the washing liquid used for backwashing can also be water, or nitrogen can be used for washing to reduce the introduction of complex components in the system. The flow rate of the washing liquid for backwashing can be 0.5 to 2 m / s.

[0045] The remaining first remaining material in the first separation device after the above steps includes a second part of the organic phase, an aqueous phase, and a solid catalyst phase.

[0046] The method of the present invention further includes performing first heating evaporation on the first remaining material, so that a first gas-phase mixture of all the second part of the organic phase, part of the aqueous phase, and unreacted raw material gas is separated from the top of the first separation device. The temperature of this first heating evaporation is 60 to 82 °C, such as 65 °C, 68 °C, 69 °C, 70 °C, 71 °C, 75 °C or 79 °C, and the pressure can be -0.1 kPa to -0.1 MPa. The first heating device can be a heating jacket arranged around the first separation device. The temperature range of the present invention can evaporate the remaining organic phase and raw material gas in the first separation device, reduce the complexity of the types of remaining materials in the first separation device, and is beneficial to simplifying the operation of further separating the solid catalyst.

[0047] The second part of the organic phase includes cyclohexane, whose boiling point is 80.7 °C. During the heating process of the first separation device, cyclohexane and water can form an azeotrope, and the azeotropic point can be 69 °C. Therefore, when the top gas phase temperature of the first separation device reaches the azeotropic point of cyclohexane and water, which is 69 °C, the azeotrope is discharged from the first separation device in the form of a first gas phase mixture and enters the cooling device. It can be seen that the formation of the azeotrope can reduce the heating energy consumption and improve the evaporation efficiency. The heating temperature range in the first separation device can be preferably 60-70 °C to ensure that the organic phase removal efficiency in the first separation device can reach more than 95%. When the pressure in the first separation device is -0.1 kPa to -0.1 MPa, the organic phase removal rate can reach 100%, thereby reducing the environmental pollution and personnel poisoning hazards in subsequent operations.

[0048] The above first gas phase mixture is condensed by the cooling device and then enters the material receiving device. In the method of the present invention, the organic phase contained in the production materials of the organic chemical process is completely recovered into the material treatment device for further treatment and recovery, reducing raw material loss and resource waste.

[0049] In one embodiment, the raw material gas can be the unreacted hydrogen in the liquid-phase benzene hydrogenation reaction. Specifically, benzene and cyclohexane in the first gas phase mixture can be condensed into liquid benzene and liquid cyclohexane, and the unreacted raw material gas (hydrogen) remains as a gas.

[0050] The remaining second residual material in the first separation device after the above first heating and evaporation treatment includes the remaining water phase and the solid catalyst phase. Due to the addition of sufficient aqueous extraction liquid, the remaining water phase and the solid catalyst phase maintain good fluidity. The second residual material is discharged from the bottom of the first separation device to the second separation device, and the discharged second residual material can obtain the solid catalyst and the water phase through solid-liquid separation. If no aqueous extraction liquid is added or the added aqueous extraction liquid is too little, after the first separation device performs heating and evaporation, the solid catalyst in the second residual material will dry and solidify at the bottom of the first separation device, making it difficult to discharge.

[0051] According to one embodiment, the solid-liquid separation of the discharged second residual material can be carried out by pressure filtration separation. Preferably, the pressure for separating the solid catalyst and the water phase by pressure filtration can be 0.5-1.0 MPa, and the filter press can be a filter cloth or filter net with a pore size of 140-160 microns (for example, 150 microns).

[0052] According to another embodiment, the solid-liquid separation of the discharged second residual material can be carried out by sedimentation evaporation separation. After the second residual material is sedimented and phase-separated in the second separation device to form a water phase and a solid catalyst phase, the water phase is discharged, and the solid catalyst phase is subjected to a second heating and evaporation to obtain the solid catalyst and a second gas phase mixture.

[0053] The second heating and evaporation can be achieved by using the second heating device on the sedimentation evaporation device. Specifically, the second heating device can be a heating jacket. The second heating and evaporation temperature can be 90-100 °C to fully evaporate the aqueous phase and organic phase entrained in the solid catalyst phase to form a second gas mixture. The generated second gas mixture enters the material receiving device after being condensed by the cooling device.

[0054] The density of the solid catalyst used in the organic chemical process is usually much greater than that of water. The methods of separating the solid catalyst and the aqueous phase by pressure filtration separation or sedimentation evaporation are simple in operation, good in separation effect, and the solid catalyst separated from the aqueous phase has a clean surface, which is beneficial to further treatment or recovery.

[0055] Furthermore, the material received by the material receiving device is processed to separate and recover the organic phase raw material. According to the above method, the material received in the material receiving device can contain an organic phase, an aqueous phase, and unreacted raw material gas.

[0056] In the method of the present invention, the organic phase and aqueous phase contained in the first gas mixture and the second gas mixture that enter the material receiving device after condensation are transformed into a liquid phase and form a liquid mixture, and the unreacted raw material gas is in a gas phase.

[0057] The material receiving device is suctioned by using a vacuum generating device to discharge the gas phase part therein. Specifically, a vacuum pump can be used for suction.

[0058] The remaining liquid mixture in the material receiving device is allowed to stand and separate into layers, and the organic phase and the aqueous phase are discharged respectively. The separated organic phase can be further rectified and reused, and the aqueous phase can be discharged as wastewater. The steps of recovering the organic matter in the method of the present invention are simple, the recovery efficiency is high, the residual impurities are few, and the raw material utilization rate is improved.

[0059] See Figure 1 , the present invention also provides a system for treating production materials from an organic chemical process, including:

[0060] The first separation device 1, equipped with a stirring device 11 and a first heating component 12, and used for receiving production materials and an aqueous extraction liquid. Preferably, the production materials and the aqueous extraction liquid enter the first separation device 1 from the top respectively;

[0061] The material receiving device 2, communicated with the first separation device 1, and receiving the organic phase, part of the aqueous phase, and unreacted raw material gas from the first separation device 1;

[0062] The second separation device 3, communicated with the bottom of the first separation device 1, and used for separating the remaining aqueous phase and the solid catalyst phase.

[0063] Among them, the material receiving device 2 communicates with the middle side wall of the first separation device 1 and is used to discharge the stratified organic phase from the first separation device 1. A solid-liquid separation device 21 is further provided between the material receiving device 2 and the first separation device 1 and is used to intercept the solid catalyst entrained in the discharged organic phase; and a reverse flushing pipe 22 is used to flush the solid catalyst intercepted on the solid-liquid separation device 21 back into the first separation device 1 by reverse flushing. The solid-liquid separation device 21 can adopt a filter screen or a filter. Further, the aperture of the filter screen or the filter can be 140-160 microns, such as 150 microns.

[0064] The material receiving device 2 communicates with the top of the first separation device 1 and is used to receive the first gas-phase mixture including all the remaining organic phase, part of the aqueous phase, and unreacted raw material gas. A cooling device 4 is further provided between the material receiving device 2 and the first separation device 1 and is used to condense the first gas-phase mixture. Specifically, the cooling device 4 can be a gas condenser.

[0065] The above system further includes a catalyst storage device 32 and a first aqueous phase storage device 33 that communicate with the bottom of the second separation device 3. Among them, the second separation device 3 can be a pressure filtration device A and / or a sedimentation evaporation device B equipped with a second heating component 31.

[0066] The above system further includes a vacuum generating device 5 that communicates with the top of the material receiving device 2, and an organic phase storage device 23 and a second aqueous phase storage device 24 that communicate with the bottom of the material receiving device 2, whereby complete separation of the gas phase, organic phase, and aqueous phase can be achieved.

[0067] According to the method and system for processing production materials from an organic chemical process of the present invention, the catalyst and discharged organic materials generated in the organic chemical process can be separated or recovered efficiently and with low energy consumption, improving the efficiency and economy of the production line, and reducing resource waste and environmental pollution. In particular, the method and system of the present invention can be applied to the withdrawal and replacement of deactivated catalysts and can also be applied to the recycling of non-deactivated catalysts.

[0068] The present invention has the following advantages:

[0069] Adopting a process that combines the static method, evaporation method, filtration method, or sedimentation evaporation method to effectively separate the organic material and the solid catalyst phase, reducing complex processes and separation energy consumption;

[0070] It can efficiently recover and separate the catalyst and organic materials in the production system and can be returned to the production system for recycling, improving the recovery efficiency, reducing the consumption of raw materials and resource waste, increasing the production efficiency, and reducing the economic cost.

Claims

1. A method for treating a production material from an organic chemical process, the production material comprising an initial catalyst phase and an organic phase, characterized in that The method comprises the following steps: (1) feeding the production material into a first separation device, adding an aqueous extract, stirring and mixing, and standing to separate phases, wherein after standing, the production material is separated from top to bottom into an organic phase, an aqueous phase, and a solid catalyst phase; (2) discharging a first portion of the upper organic phase from the first separation device to a material receiving device; (3) in the first separation device, performing a first heating evaporation on the first remaining material including the second organic phase, the aqueous phase and the solid catalyst phase, so that a first gas phase mixture is separated from the top of the first separation device, wherein the first gas phase mixture includes all of the second organic phase, part of the aqueous phase and unreacted raw material gas; (4) discharging a second residual material including a remaining water phase and a solid catalyst phase from the bottom of the first separation device, and separating the second residual material by filter pressing to obtain a solid catalyst and a water phase; or allowing the second residual material to settle and separate into a water phase and a solid catalyst phase, discharging the water phase, and performing a second heating evaporation on the solid catalyst phase to obtain a mixture of a solid catalyst and a second gas phase.

2. The method according to claim 1, wherein: In step (2), the first portion of organic phase separated is discharged from the first separation device to the material receiving device, and solid-liquid separation and backwashing are performed, and the solid catalyst entrained in the first portion of organic phase is recovered to the first separation device.

3. The method according to claim 1, wherein: In step (1), the weight ratio of the production material to the aqueous extract is (1-3):

1.

4. The method according to claim 1, wherein: The first gas phase mixture and the second gas phase mixture enter the material receiving device after being condensed respectively.

5. The method according to claim 4 further comprises: sucking the material entering the material receiving device to discharge the gas phase part thereof, and letting the remaining liquid phase stand for stratification and discharging it separately to obtain an organic phase and an aqueous phase.

6. The method according to claim 1, wherein: The temperature of the first heating evaporation is 60-82° C., the temperature of the second heating evaporation is 90-100° C.; the pressure of the filter press is 0.5-1.0 MPa.

7. The method according to any one of claims 1 to 6, wherein: The organic chemical process is a liquid phase benzene hydrogenation process.

8. The method according to claim 7, wherein: The aqueous extract is water, the organic phase includes benzene and cyclohexane, the raw material gas is hydrogen, the catalyst in the initial catalyst phase is a deactivated catalyst, and the backwashing is water washing.

9. A system for treating a production material from an organic chemical process, the production material comprising an initial catalyst phase and an organic phase, characterized in that: The system includes, in order according to the flow direction of production materials: A first separation device, equipped with a stirring device and a first heating component, for receiving the production material and the aqueous extract; a material receiving device, connected to the first separation device, and receiving the organic phase, part of the aqueous phase and unreacted raw material gas from the first separation device; The second separation device is connected to the bottom of the first separation device and is used to separate the residual water phase and the solid catalyst phase.

10. The system according to claim 9, wherein: The material receiving device is communicated with the middle side wall of the first separation device, and is used for receiving the organic phase discharged from the first separation device.

11. The system according to claim 9, wherein: Between the material receiving device and the middle side wall of the first separating device is provided: A solid-liquid separation device for intercepting the solid catalyst entrained in the discharged organic phase; A back flushing pipe is used to flush the retained solid catalyst back into the first separation device.

12. The system according to claim 9, wherein: The material receiving device is communicated with the top of the first separation device and is used for receiving a first gas phase mixture including all the remaining organic phase, part of the water phase and unreacted raw material gas.

13. The system according to claim 9, further comprising a cooling device disposed between the material receiving device and the top of the first separation device, for condensing the material entering therein.

14. The system of claim 9, further comprising a catalyst storage device and a first water phase storage device in communication with a bottom of the second separation device.

15. The system according to claim 9, wherein: The second separation device is a filter press and / or a sedimentation evaporation device.

16. The system according to claim 9, further comprising a vacuum generating device connected to the top of the material receiving device, and an organic phase storage device and a second aqueous phase storage device connected to the bottom of the material receiving device.

17. The system of claim 11, wherein: The solid-liquid separation device is a filter screen or a filter.

Citation Information

Patent Citations

  • Method for recovering catalyst in preparation of cyclohexene by partial hydrogenation of benzene

    CN102161008B