Intermittent methylaluminoxane / modified methylaluminoxane production and separation combined system

Abstract

The utility model discloses an intermittent methylaluminoxane / modified methylaluminoxane production and separation combined system which comprises a reaction kettle for reaction, a filtering, washing and drying machine for post-processing solid-liquid products obtained by reaction, a waste liquid tank for collecting washing liquid of the filtering, washing and drying machine, and a product solution tank for collecting products, the vacuum rectifying tower is used for collecting gas products obtained by reaction; and the return tank is used for collecting gas in the vacuum rectifying tower. According to the utility model, a reduced-pressure rectification mode is adopted, the temperature of the bottom of the rectification tower is reduced, the temperature of the whole system is ensured to be within the allowable range of physical properties of reaction materials, and meanwhile, the evaporated aluminum alkyl is recovered through rectification, so that the risk caused by leakage of the aluminum alkyl is reduced to the greatest extent. The device disclosed by the utility model is simple in process flow, relatively high in reaction yield, relatively low in reaction danger level and relatively high in production safety coefficient.

Description

Technical Field

[0001] The utility model relates to an intermittent methylaluminoxane / modified methylaluminoxane production and separation combined system, belonging to the technical field of chemical reaction system equipment. Background Art

[0002] Methylaluminoxane and modified methylaluminoxane are highly efficient co-catalysts in metallocene and late transition metal olefin polymerization catalysts with high catalytic activity. Metallocene catalysts used in the synthesis of new materials such as metallocene polyolefins, metallocene polyolefin elastomers, metallocene polyolefin lubricants (PAO) and metallocene polyolefin waxes, new materials cyclic polyolefins (COC / COP) all require them as co-catalysts.

[0003] Compared with traditional PE materials, metallocene polyethylene has a narrower molecular weight distribution and a regular molecular chain structure. This is reflected in the product performance. Metallocene polyethylene has high mechanical strength and good optical properties. Compared with traditional polypropylene products, metallocene polypropylene has the characteristics of narrow relative molecular weight distribution, low melting point, and no soluble short-chain block copolymers. The prepared products have low precipitates and good sensory properties, and can be used in the fields of medical and health care and food packaging. At the same time, the large-scale industrialization of polyolefin elastomers (POE) and the industrialization of high sterically hindered cyclic olefin polymers (COC / COP) fully reflect the application prospects of metallocene olefin polymerization catalysts!

[0004] The development of metallocene polyolefins depends on the continuous improvement and large-scale industrial production of metallocene catalysts and their co-catalysts - methylaluminoxane and modified methylaluminoxane. Unfortunately, the high-efficiency co-catalysts methylaluminoxane and modified methylaluminoxane cannot be produced domestically and are all imported from foreign companies, resulting in high costs for metallocene catalysts and relatively high prices for metallocene polyolefins and their products, which are difficult for the terminal to accept. This has also become a major bottleneck problem for the mass production of metallocene polyolefins.

[0005] There are many methods for synthesizing methylaluminoxane and modified methylaluminoxane. According to the different forms of water involved in the reaction, they can be summarized into two categories: indirect water process and direct water process. The two synthesis processes have their own advantages and disadvantages: the indirect water process disperses various water carriers (such as hydrated inorganic salts, etc.) into organic solvents and then reacts with trimethylaluminum-triisobutylaluminum solution. The reaction process is relatively mild, the requirements for equipment are low, and the production process is safer, but the single-pass yield of the target product methylaluminoxane and modified methylaluminoxane is not high, about 40%; the direct water process uses different reactant feeding technologies to add controlled free water to the toluene solution of trimethylaluminum-triisobutylaluminum. Since the trimethylaluminum-triisobutylaluminum system reacts very violently with water, the safety risk of the process is relatively large and the requirements for equipment are relatively high, but the yield of methylaluminoxane and modified methylaluminoxane can reach more than 50%. Summary of the invention

[0006] The technical problem to be solved by the utility model is to provide an intermittent production and separation combined system for producing methylaluminoxane and modified methylaluminoxane.

[0007] The utility model solves the above technical problems through the following technical solutions:

[0008] An intermittent methylaluminoxane / modified methylaluminoxane production and separation combined system, comprising:

[0009] A reactor for reaction, wherein a reaction solution feed port, a gas outlet, and an emulsion feed port are provided on the top of the reactor, and an outlet is provided on the bottom, the reaction solution feed port is connected to a plurality of reaction solution feed lines through a mixing feed line, and the emulsion feed port is connected to the emulsion feed line;

[0010] A filter, washing and drying machine for post-processing the solid and liquid products obtained by the reaction, wherein the filter, washing and drying machine is provided with a feed port and a washing water inlet at the top, a solid discharge port at the bottom, and a liquid outlet at the bottom, the feed port is connected with the discharge port of the reactor, the washing water inlet is connected with the washing water feed line, the solid discharge port is connected with the solid barrel, and the liquid outlet is connected with the liquid outlet line;

[0011] A waste liquid tank for collecting and filtering the washing liquid of the washing and drying machine, wherein the waste liquid tank has a feed inlet at the top and a discharge outlet at the bottom, the feed inlet is connected to the liquid outlet line, and the discharge outlet is connected to the waste liquid outlet device line;

[0012] A product solution tank for collecting the product, wherein the top of the product solution tank is provided with a feed inlet, the bottom of the product solution tank is provided with a discharge port, and the feed inlet is connected to the liquid outlet line;

[0013] A vacuum distillation tower for collecting the gaseous products obtained by the reaction, wherein the vacuum distillation tower is provided with a gas outlet at the top, a feed inlet in the middle, and a discharge inlet at the bottom, and the feed inlet is connected to the gas outlet of the reactor;

[0014] A reflux tank is used to collect gas in a vacuum distillation tower. A feed port is provided at the top of the reflux tank, and a liquid outlet is provided at the bottom. The feed port is connected to the gas outlet of the vacuum distillation tower, and the liquid outlet is connected to the C4 outlet line.

[0015] Preferably, a reaction solution cooler is provided between the mixed feed line and the reaction solution feed port of the reactor; an emulsion cooler is provided between the emulsion feed line and the emulsion feed port of the reactor; a jacket for cooling the reactor is provided outside the reactor, and a refrigerant inlet and a refrigerant outlet (the refrigerant temperature is not greater than -20°C) are provided on the jacket; a reflux port is also provided at the top of the reactor, which is connected to the discharge port of the vacuum distillation tower. The reactor adopts intermittent operation, the reactants are in the form of solution, and the deionized water participating in the reaction adopts a low-concentration emulsion mixed with a solvent.

[0016] More preferably, the reflux port of the reactor is connected to the discharge port of the vacuum distillation tower via a vacuum distillation tower bottom pump.

[0017] Preferably, a vent is also provided on the top of the filter, washing and drying machine, which is connected to the vent main pipe through a vacuum pump.

[0018] Preferably, the filter-washer-dryer is provided with a jacket for heating the filter-washer-dryer, and the jacket is provided with a heat medium inlet and a heat medium outlet.

[0019] Preferably, the discharge port of the waste liquid tank is connected to the waste liquid discharge device line through a waste liquid pump; the waste liquid tank is also provided with a vent, which is connected to the vent main pipe.

[0020] Preferably, the discharge port of the product solution tank is connected to a product solution booster pump (the product temperature is not greater than 10° C.); the product solution tank is also provided with a vent, which is connected to a vent main pipe.

[0021] Preferably, a reboiling device is provided at the bottom of the vacuum distillation tower, which includes a reboiler forming a loop with the vacuum distillation tower through a pipeline. The heat source of the reboiler and the filter washing and drying machine is steam with a pressure of not less than 8 kg.

[0022] Preferably, a vacuum distillation tower top cooler is provided between the gas outlet of the vacuum distillation tower and the feed port of the reflux tank; a reflux port is also provided at the upper part of the vacuum distillation tower, and the reflux port is connected with the liquid outlet of the reflux tank; the reflux tank is also provided with a vent port, which is connected with the vent main pipe through a second vacuum pump.

[0023] More preferably, the liquid outlet of the reflux tank is connected to the reflux port of the vacuum distillation tower through a vacuum distillation tower reflux pump.

[0024] The utility model can control the feed rate and increase related facilities to reduce the risk of direct water process and improve the safety factor of production while producing methylaluminoxane and modified methylaluminoxane. The utility model adopts vacuum distillation to reduce the bottom temperature of the distillation tower, ensure that the temperature of the entire system is within the allowable range of the physical properties of the reaction materials, and recover the evaporated alkyl aluminum through distillation to minimize the risk of alkyl aluminum leakage. Compared with the prior art, the concentration of the product obtained by the utility model is not less than 17wt%; the reaction conditions are mild, the reaction temperature is -10℃~10℃, and the reaction pressure is ≤0.1MPa. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 The utility model provides a schematic diagram of the methylaluminoxane / modified methylaluminoxane production and separation combined system. DETAILED DESCRIPTION

[0026] In order to make the present invention more obvious and easy to understand, preferred embodiments are described in detail as follows in conjunction with the accompanying drawings.

[0027] Example

[0028] like Figure 1 As shown, the utility model provides an intermittent methylaluminoxane / modified methylaluminoxane production and separation combined system, comprising:

[0029] Reactor 1: A gas outlet is provided at the top of the reactor 1; two feed ports are provided on one side of the upper part of the reactor 1, namely, a reactant solution feed port and an emulsion feed port, and the reactant solution feed port is connected to the outlet of the reactant solution cooler 16 through a pipeline 1 21; a reflux port is provided on the other side of the upper part of the reactor 1; the emulsion feed port is connected to the outlet of the emulsion cooler 17 through a pipeline 2 23, and a dedicated nozzle is provided at the inlet end of the emulsion at the bottom of the reactor 1 for discharging; a discharge port is provided at the bottom of the reactor 1, which is connected to the feed port of the filter washing and drying machine 2 through a pipeline 11 25; the gas outlet is connected to the feed port of the vacuum distillation tower 4 through a pipeline 9 24; a jacket is provided on the outside of the reactor 1, a refrigerant inlet is provided at the bottom of the jacket, which is connected to the pipeline 8 47, and a refrigerant outlet is provided at the upper part, which is connected to the pipeline 7 48;

[0030] Reactant solution cooler 16: The shell side inlet of the reactant solution cooler 16 is connected to the reaction solution feed line 1 18 and the reaction solution feed line 2 19 respectively through the mixed feed line 20; the shell side outlet is connected to the reactant solution feed port of the reactor 1 through the pipeline 1 21; the tube side of the reactant solution cooler 16 uses a refrigerant, and the feed port and the discharge port are connected to the pipeline 4 53 and the pipeline 3 54 respectively;

[0031] Emulsion cooler 17: The shell side inlet of the emulsion cooler 17 is connected to the emulsion feed line 22, and the shell side outlet is connected to the emulsion feed port of the reactor 1 through the pipeline 2 23; the tube side of the emulsion cooler 17 runs the refrigerant, and the feed port and the discharge port are connected to the pipeline 6 51 and the pipeline 5 52 respectively;

[0032] Filtering, washing and drying machine 2: A feeding port is provided at the top of the filtering, washing and drying machine 2, which is connected to the discharging port of the reactor 1 through the pipeline 11 25; a vent is provided on one side of the top, which is connected to the inlet of the vacuum pump 3 through the pipeline 12 26; a washing water inlet is provided on the other side, which is connected to the washing water feeding line 38; a solid discharging port is provided at the bottom of the side of the filtering, washing and drying machine 2, which is connected to the solid barrel 15 through the pipeline 16 39; a discharging port is provided at the bottom, which is connected to the pipeline 20 29 through the liquid outlet line 28; a jacket is provided on the outside of the filtering, washing and drying machine 2, a heat medium inlet is provided on the upper part of the jacket, which is connected to the pipeline 14 49, and a heat medium outlet is provided on the lower part, which is connected to the pipeline 15 50;

[0033] Vacuum pump 1 3: The inlet of vacuum pump 1 3 is connected to the venting port at the top of the filter washing and drying machine 2 through pipeline 12 26; the outlet of vacuum pump 1 3 is connected to the venting main pipe 42 through pipeline 13 27;

[0034] Solid material barrel 15: a feed port is provided at the top, which is connected to the solid material discharge port of the filter washing and drying machine 2 through pipeline 16 39;

[0035] Product solution tank 11: A feed port is provided on one side of the upper part of the product filtrate tank 11, which is connected to the liquid outlet line 28 through pipeline 20 29; a vent port is provided on the other side, which is connected to the vent main pipe 42 through pipeline 21 65; a discharge port is provided on the lower part, which is connected to the inlet of the product solution booster pump 12 through pipeline 23 30;

[0036] Product solution booster pump 12: the inlet of the product solution booster pump 12 is connected to the discharge port of the product solution tank 11 through pipeline 23 30; the outlet of the product solution booster pump 12 is connected to the product outlet line 32 through pipeline 22 31;

[0037] Vacuum distillation tower 4: The top of the vacuum distillation tower 4 is provided with an air outlet, one side of the middle is provided with a feed port, the bottom is provided with a discharge port, and one side of the upper part is provided with a reflux port. The feed port of the vacuum distillation tower 4 is connected to the air outlet of the reactor 1 through a pipeline 9 24, and the discharge port of the vacuum distillation tower 4 is connected to the vacuum distillation tower bottom pump 10 through a pipeline 10 34 and the reflux port of the reactor 1; the bottom of the vacuum distillation tower 4 is connected to a heat source, i.e., a reboiler 9, through a pipeline 26 59 and a pipeline 25 60 to form a loop;

[0038] Vacuum distillation tower top cooler 5: the shell side inlet of the vacuum distillation tower top cooler 5 is connected to the gas outlet of the vacuum distillation tower 4 through pipeline twenty-nine 35, and the shell side outlet is connected to the feed port of the reflux tank 6 through pipeline thirty-three 36; the tube side of the vacuum distillation tower top cooler 5 uses refrigerant;

[0039] Reflux tank 6: The top of reflux tank 6 is provided with a feed port and a gas outlet, and the bottom is provided with a liquid outlet. The gas outlet of vacuum distillation tower 4 is connected with the feed port of reflux tank 6 through vacuum distillation tower top cooler 5, the gas outlet of reflux tank 6 is connected with the inlet of vacuum pump 2 7 through pipeline 34 37, and the liquid outlet of reflux tank 6 is connected with pipeline 30 40 and C4 outlet line 41 at the reflux port of vacuum distillation tower 4 through vacuum distillation tower top reflux pump 8;

[0040] Vacuum pump 2 7: The inlet of vacuum pump 2 7 is connected to the gas outlet of reflux tank 6 through pipeline 34 37, and the outlet of vacuum pump 2 7 is connected to vent main pipe 42 through pipeline 35 38;

[0041] Reboiler 9: The shell side inlet of the reboiler 9 is connected to the bottom of the vacuum distillation tower 4 through pipeline 26 59 (that is, it is connected to the liquid that needs to be reboiled at the bottom of the reboiler 9), and the shell side outlet is connected to the bottom of the vacuum distillation tower 4 through pipeline 25 60; the tube side of the reboiler 9 passes the heat medium, and the inlet and outlet are connected to the heat medium through pipeline 27 57 and pipeline 28 58 respectively;

[0042] Vacuum distillation tower bottom pump 10: the inlet of the vacuum distillation tower bottom pump 10 is connected to the discharge port of the vacuum distillation tower 4 through the pipeline twenty-four 33, and the outlet is connected to the reflux port of the reactor 1 through the pipeline ten 34;

[0043] Vacuum distillation tower top cooler 5: the shell side inlet of the vacuum distillation tower top cooler 5 is connected to the gas outlet of the vacuum distillation tower 4 through pipeline twenty-nine 35, the shell side outlet is connected to the reflux tank 6 through pipeline thirty-three 36, the tube side of the vacuum distillation tower top cooler 5 uses refrigerant, and the refrigerant inlet and refrigerant outlet are connected to pipeline thirty-one 55 and pipeline thirty-two 56 respectively;

[0044] Waste liquid tank 13: A feed port is provided on one side of the upper portion of the waste liquid tank 13, which is connected to the liquid outlet line 28 through pipeline 18 43; a vent port is provided on the other side, which is connected to the vent main pipe 42 through pipeline 17 46; a discharge port is provided on the lower portion, which is connected to the inlet of the waste liquid pump 14 through pipeline 19 44;

[0045] Waste liquid pump 14: The inlet of the waste liquid pump 14 is connected to the discharge port of the waste liquid tank 13 through pipeline 19 44, and the outlet of the waste liquid pump 14 is connected to the waste liquid outlet line 45.

[0046] The utility model adopts a kettle reactor, and two reactant inlets are arranged on the top of the reactor, one of which is an inlet for a solution mixed with reactants and solvents, which enters the reactor after being cooled to 0°C by a cooler; the other is an emulsion composed of a mixture of desalted water and solvent, which enters the reactor after being cooled to 0°C by a cooler; the process is a direct water method, and the reactant solution needs to be added to the reactor first, and then the emulsion is added to react, and the amount and speed of the emulsion added determine the intensity of the reaction. Before the reaction, the desalted water and the solvent are mixed according to a certain concentration ratio to prepare an emulsion, and then the concentration of the reaction water is diluted, and the intensity of the reaction is limited by controlling the flow rate added per unit time. At the same time, a special atomizing nozzle for the emulsion is arranged in the reactor. Under the action of the special atomizing nozzle, the emulsion is cut into particles with a diameter of 10 to 150 microns and injected into the reactor, which further reduces the intensity of the reaction compared with the traditional millimeter-level nozzle. The reaction solution and reaction emulsion are precooled to 0°C before entering the reactor. The reactor jacket only needs to adjust and control the heat released by the reaction to control the temperature of the entire reaction stage at around 0°C, further reducing the degree of reaction.

[0047] The integrated filtering, washing and drying machine is used to combine the filtering, washing and drying processes on the same equipment, which can minimize the process that hazardous materials go through and reduce the risk level of the entire reaction. The filtration uses a high-precision filter screen to intercept solid materials with a particle size of more than 10μm. The filtration process can be combined with vacuum operation to recover the filtrate to the greatest extent, effectively realizing solid-liquid separation. The filter cake is flat during filtration and the solid-liquid separation effect is good. There may be residual components of alkyl aluminum and aluminoxane in the remaining filter cake. In order to prevent the alkyl aluminum and aluminoxane entrained in the solid from being brought out of the system and encountering air during the discharge of the solid matter, these components are balanced by water washing before the solid matter is discharged. There is a 360° rotating spray device on the inside of the filter, so that the cleaning (washing) liquid is evenly distributed in the container, which can realize the cleaning of the container interior and the paddle washing of the material. The filter cake and the washing liquid are mixed by stirring with lifting blades, so that the remaining filter cake is fully washed. Two channels are set up through automatic control, one for sending the reaction filtrate into the reaction solution tank, and the other for sending the washing waste liquid after washing to the waste liquid tank; the remaining filter cake after filtration is scraped loose layer by layer by the stirring blade, and the equipment heating device heats the filter cake evenly. Under the vacuum state, the integrated machine has its own jacket to pass heating steam to heat the wet material, accelerate evaporation, and achieve the purpose of drying; the dried material is scraped loose by the stirring blade, and then automatically discharged from the side discharge port of the tank wall by the stirring blade.

[0048] Usually, during the synthesis of methylaluminoxane and modified aluminoxane, methane and isobutane are produced. Methane and isobutane are discharged in the form of gas phase during the reaction process. At the same time, a small amount of gaseous trimethylaluminum is discharged along with methane and isobutane. In order to prevent the potential danger caused by trimethylaluminum, a distillation tower is set on the top of the reactor to recover the gaseous trimethylaluminum and send it back to the reactor. At the same time, the methane and isobutane produced by the reaction are separated, and isobutane is recovered separately. The distillation adopts the method of reducing pressure. A vacuum pump is set after the reflux tank at the top of the distillation tower. The vacuum degree is controlled at 15-50kPa (a) to ensure that the temperature of the whole tower is controlled within the suitable range of trimethylaluminum, triisobutylaluminum and modified aluminoxane, further reducing the risk of the reaction, so that the whole reaction can be carried out in a relatively mild environment.

Claims

1. An intermittent methylaluminoxane / modified methylaluminoxane production and separation combined system, characterized in that: include: A reaction kettle (1) for reaction, wherein the top of the reaction kettle (1) is provided with a reaction solution feed port, a gas outlet, and an emulsion feed port, and the bottom is provided with an outlet, the reaction solution feed port is connected to a plurality of reaction solution feed lines via a mixing feed line (20), and the emulsion feed port is connected to an emulsion feed line (22); A filter, washing and drying machine (2) for post-processing the solid and liquid products obtained by the reaction, wherein the filter, washing and drying machine (2) is provided with a feed port and a washing water inlet at the top, a solid discharge port at the bottom, and a liquid outlet at the bottom, the feed port is connected to the discharge port of the reaction kettle (1), the washing water inlet is connected to the washing water feed line (38), the solid discharge port is connected to the solid material barrel (15), and the liquid outlet is connected to the liquid outlet line (28); A waste liquid tank (13) for collecting washing liquid from the filter washing and drying machine (2), wherein the waste liquid tank (13) is provided with a feed inlet at the top and a discharge outlet at the bottom, the feed inlet being connected to a liquid outlet line (28), and the discharge outlet being connected to a waste liquid outlet line (45); A product solution tank (11) for collecting the product, wherein the top of the product solution tank (11) is provided with a feed inlet, the bottom of the product solution tank (11) is provided with a discharge port, and the feed inlet is connected to a liquid outlet line (28); A vacuum distillation tower (4) for collecting the gaseous product obtained by the reaction, wherein the vacuum distillation tower (4) is provided with a gas outlet at the top, a feed inlet in the middle, and a discharge inlet at the bottom, and the feed inlet is connected to the gas outlet of the reaction kettle (1); A reflux tank (6) is used to collect gas in a vacuum distillation tower (4). The top of the reflux tank (6) is provided with a feed port, and the bottom is provided with a liquid outlet. The feed port is connected to the gas outlet of the vacuum distillation tower (4), and the liquid outlet is connected to a C4 outlet line (41).

2. The intermittent methylaluminoxane / modified methylaluminoxane production and separation combined system according to claim 1, characterized in that: A reaction solution cooler (16) is provided between the mixed feed line (20) and the reaction solution feed port of the reactor (1); an emulsion cooler (17) is provided between the emulsion feed line (22) and the emulsion feed port of the reactor (1); a jacket for cooling the reactor (1) is provided outside the reactor (1), and a refrigerant inlet and a refrigerant outlet are provided on the jacket; a reflux port is also provided at the top of the reactor (1), which is connected to the discharge port of the vacuum distillation tower (4).

3. The intermittent methylaluminoxane / modified methylaluminoxane production and separation combined system according to claim 2, characterized in that: The reflux port of the reaction kettle (1) is connected to the discharge port of the vacuum distillation tower (4) via a vacuum distillation tower bottom pump (10).

4. The intermittent methylaluminoxane / modified methylaluminoxane production and separation combined system according to claim 1, characterized in that: The top of the filter, washing and drying machine (2) is also provided with a venting port which is connected to the venting main pipe (42) via a vacuum pump (3).

5. The intermittent methylaluminoxane / modified methylaluminoxane production and separation combined system according to claim 1, characterized in that: The filter, washing and drying machine (2) is provided with a jacket for heating the filter, washing and drying machine (2), and the jacket is provided with a heat medium inlet and a heat medium outlet.

6. The intermittent methylaluminoxane / modified methylaluminoxane production and separation combined system according to claim 1, characterized in that: The discharge port of the waste liquid tank (13) is connected to the waste liquid discharge device line (45) through the waste liquid pump (14); the waste liquid tank (13) is also provided with a venting port, which is connected to the venting main pipe (42).

7. The intermittent methylaluminoxane / modified methylaluminoxane production and separation combined system according to claim 1, characterized in that: The discharge port of the product solution tank (11) is connected to the product solution booster pump (12); the product solution tank (11) is also provided with a venting port, which is connected to the venting main pipe (42).

8. The intermittent methylaluminoxane / modified methylaluminoxane production and separation combined system according to claim 1, characterized in that: A reboiler is provided at the bottom of the vacuum distillation tower (4), which comprises a reboiler (9) which forms a loop with the vacuum distillation tower (4) through a pipeline.

9. The intermittent methylaluminoxane / modified methylaluminoxane production and separation combined system according to claim 1, characterized in that: A vacuum distillation tower top cooler (5) is provided between the gas outlet of the vacuum distillation tower (4) and the feed inlet of the reflux tank (6); a reflux port is also provided at the top of the vacuum distillation tower (4), and the reflux port is connected to the liquid outlet of the reflux tank (6); the reflux tank (6) is also provided with a vent port, which is connected to the vent main pipe (42) through a second vacuum pump (7).

10. The intermittent methylaluminoxane / modified methylaluminoxane production and separation combined system according to claim 9, characterized in that: The liquid outlet of the reflux tank (6) is connected to the reflux port of the vacuum distillation tower (4) through a vacuum distillation tower reflux pump (8).

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