A production process and system for polyketone resin

Abstract

The present invention relates to the field of chemical production technology, and in particular to a production process and system for polyketone resin. The present invention further improves the mass transfer and heat transfer effects by coordinating the temperature control, stirring and external circulation heat exchange in the reaction kettle during the reaction process, so that the temperature of the slurry material in the reaction kettle is maintained within an appropriate range, thereby avoiding the degradation of the quality of the polyketone resin caused by heat transfer problems; by setting a slurry washing process, the catalyst precious metals wrapped on the surface and inside of the polyketone resin are fully washed into the washing medium, which greatly reduces the residual amount of the catalyst precious metals in the obtained polyketone resin, and can fully recover the precious metals, the system runs stably, is easy to operate, and has good economic benefits.

Description

Technical Field

[0001] The invention relates to the technical field of chemical production, and in particular to a production process and system for a polyketone resin. Background Art

[0002] Polyketone (POK) is an emerging environmentally friendly material that can be used in electronics, automobiles, aerospace, machinery, food packaging, fiber and other fields. It is a new type of green polymer material formed by the copolymerization of carbon monoxide and olefins (ethylene, propylene). Its main molecular chain is a tight crystalline structure formed by carbon and hydrogen, which makes it have better chemical resistance, hydrolysis resistance, impact resistance, friction resistance and high barrier properties than conventional engineering plastics. For example, its impact strength is 230% higher than that of nylon and PBT. According to its different application scenarios, the molecular weight is usually adjusted between 50,000 and 500,000.

[0003] Slurry polymerization is mainly used in the industrial production of polyketone. This process has certain advantages in the polymerization catalytic activity, molecular weight and distribution of polyketone, and mainly includes precipitation, washing, filtration, drying and residual liquid distillation recovery process. In the slurry polymerization process, the molecular weight distribution and melt index of polyketone resin are often increased. It is usually believed that there is a problem with the reaction itself or the catalyst, so the reactants, reaction temperature and pressure are closely monitored and adjusted, or the catalyst is replaced, but the problem is often not solved. In addition, palladium-based precious metal catalysts are required in the polymerization process. Slurry polymerization causes the catalyst to be embedded in the polymer and difficult to recover, which increases production costs.

[0004] In patents CN1018734B and CN1008102B, methanol or a mixture of methanol and phosphine ligands is used to wash the polyketone resin, which can remove up to 80% of the palladium in the resin, but the palladium content remaining in the polyketone is still considerable.

[0005] Therefore, it is of great significance to develop a polyketone resin production process that can strictly control the molecular weight distribution and melt index, has low palladium residue in the product, and can recover precious metals. Summary of the invention

[0006] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a production process and system for a polyketone resin, which has the characteristics of uniform mass and heat transfer in the reaction stage, low palladium residue in the product, and recoverable precious metals.

[0007] The first aspect of the present invention provides a production process of a polyketone resin, comprising the following steps:

[0008] Reaction process: adding suspension medium, catalyst, seed and reaction monomer into the reaction device, controlling reaction temperature and reaction pressure, stirring the reaction materials in the reaction device during the reaction, and performing external circulation heat exchange on the reaction materials; the external circulation heat exchange includes continuously leading out the reaction materials in the reaction device, exchanging heat, and then transporting them to below the liquid level of the reaction materials in the reaction device;

[0009] Slurry washing step: washing the slurry containing polyketone with a washing medium to obtain a washed slurry; the washing temperature is 30-80°C;

[0010] Solid-liquid separation step: performing solid-liquid separation on the washed slurry to obtain a solid and a liquid containing a polyketone resin;

[0011] Drying process: Dry the solid containing the polyketone resin to obtain polyketone resin powder or granules.

[0012] In some embodiments of the present invention, the production process of the polyketone resin further comprises one or more of a monomer recovery process, a granulation process, a solvent recovery process, a solvent distillation and purification process, and a precious metal recovery process;

[0013] The monomer recovery process comprises: after the reaction is completed, the material in the reaction device is transported to the monomer recovery device, and is separated into a volatile phase containing the monomer and a slurry from which the monomer is removed, and then the volatile phase containing the monomer is subjected to gas-liquid separation, the obtained gas is returned to the reaction device, and the slurry from which the monomer is removed is transported to a slurry washing process;

[0014] The granulation process uses the polyketone resin powder or particles obtained in the drying process as raw materials, and granulates them through a granulation device to obtain polyketone resin particles;

[0015] The solvent recovery step recovers the liquid obtained in the solid-liquid separation step and the moisture collected in the drying step, a part of which is reused in the slurry washing step, and the rest is distilled and purified;

[0016] The solvent distillation and purification process separates and purifies the recovered solvent by distilling the recovered solvent to obtain light components, intermediate components and heavy components;

[0017] The precious metal recovery step is to enrich the precious metals in the heavy components obtained after the recovery solvent is distilled and purified in the process, so as to achieve the recovery of precious metals.

[0018] A second aspect of the present invention provides a polyketone resin production system, comprising a reaction unit, a slurry washing unit, a centrifugal unit and a drying unit;

[0019] The reaction unit comprises a reactor for reacting to generate a slurry containing polyketone; a stirring assembly for stirring the slurry material is arranged inside the reactor, an external circulation pipeline communicating with the inside of the reactor is arranged outside the reactor, a material outlet of the external circulation pipeline is arranged at the lower part of the side wall of the reactor, and the homogenization and temperature control of the material in the reactor are achieved through the external circulation pipeline;

[0020] The slurry washing unit comprises a slurry washing kettle, which is provided with a slurry inlet containing polyketone and a washing medium adding inlet, and is used to wash the surface of the polyketone and the palladium wrapped inside into the washing medium to obtain a mixed material consisting of the washed slurry and the washing medium;

[0021] The solid-liquid separation unit comprises a solid-liquid separation device, the feed inlet of the solid-liquid separation device is connected to the mixed material outlet of the slurry washing kettle, and is used for solid-liquid separation of the mixed material to obtain a solid phase containing polyketone and a clear liquid;

[0022] The drying unit comprises a drying device for drying the solid phase containing polyketone to obtain polyketone resin powder or particles.

[0023] In some embodiments of the present invention, the polyketone resin production system further comprises one or more of a monomer recovery unit, a granulation unit, a solvent recovery unit, a solvent distillation and purification unit, and a precious metal recovery unit;

[0024] The monomer recovery unit comprises a monomer recovery tank, wherein the top of the monomer recovery tank is provided with a material inlet and a volatile phase outlet containing monomers, the side is provided with a liquid phase inlet, and the bottom is provided with a slurry outlet for removing monomers; the material inlet is connected with the material outlet at the bottom of the reactor, so that the material obtained by the reaction enters the monomer recovery tank and is separated into a volatile phase containing monomers and a slurry for removing monomers; the outside of the monomer recovery tank is provided with a gas-liquid separation device connected with the inside of the monomer recovery tank, which is used for gas-liquid separation of the volatile phase containing monomers;

[0025] The granulation unit includes a granulator for preparing polyketone resin particles from the polyketone resin powder or particles obtained in the drying process;

[0026] The solvent recovery unit comprises a solvent recovery tank, the inlet of the solvent recovery tank is respectively connected to the liquid outlet of the solid-liquid separation device and the solvent outlet of the drying device, and the solvent recovery tank is provided with two outlets, one outlet is connected to the washing medium inlet of the slurry washing kettle, and the other outlet is connected to the feed inlet of the solvent distillation device in the system;

[0027] The solvent distillation and purification unit comprises a solvent distillation tower, the feed port of which is connected to the outlet of the solvent recovery device in the system, and is used to distill the recovered solvent, the tower top is provided with a light component outlet, the tower bottom is provided with a heavy component outlet, and the middle of the tower is provided with an intermediate component outlet;

[0028] The precious metal recovery unit comprises a heavy metal recovery device, which is used to enrich and recover the precious metals in the heavy components obtained after the solvent is distilled and purified.

[0029] Compared with the prior art, the present invention has the following beneficial effects:

[0030] 1. In the production process of polyketone resin provided by the present invention, the reaction device enhances the mass transfer and heat transfer effect of the material in the kettle through the combined action of the stirring paddle and the external circulation, and the temperature of the slurry material is maintained within an appropriate range through temperature control in the reactor and heat exchange in the external circulation, so as to achieve strict control of the reaction temperature and uniform mixing of the solid-liquid system, improve the uniformity and selectivity of the reaction, and avoid the degradation of the quality of the polyketone resin caused by heat transfer problems (because the molecular weight distribution and melt index of the polyketone resin are greatly affected by the reaction temperature, the heat transfer and mass transfer in the slurry reaction process are uneven and untimely, and the actual reaction temperature is very likely to be too high or locally too high, resulting in degradation of the polyketone quality); in the slurry washing process, by regulating the washing temperature, the washing temperature is controlled at 30-80°C, so that the catalyst precious metals wrapped on the surface and inside of the polyketone resin can be fully washed into the washing medium, which greatly reduces the residual amount of the catalyst precious metals in the obtained polyketone resin, and the residual palladium in the polyketone resin can be as low as 1 ppm The temperature is below that of the existing polyketone resin production process, which means that the present application makes the production cost much lower than the existing technology by regulating the washing temperature, and achieves unexpected technical effects; after centrifugation, the catalyst precious metal enters the centrifugal filtrate, and finally the precious metal is enriched after distillation and concentration, which can fully recover the precious metal, reduce the production cost, and has good economic benefits.

[0031] 2. The production process of the polyketone resin provided by the present invention greatly improves the monomer utilization rate by setting up a monomer recovery process, separating the unreacted monomer from the solvent and returning the monomer to the reaction device for further reaction. The solvent recovery and reuse are achieved by setting up a solvent recovery process and a solvent distillation and purification process, thereby achieving good economic benefits.

[0032] 3. The polyketone resin production system provided by the present invention realizes external circulation and temperature control of materials in the reactor by arranging an external circulation pipeline outside the reactor and arranging a compressor and a heat exchanger on the pipeline. The reaction materials after heat exchange are transported to below the reaction material liquid surface in the reaction device, promoting full mixing of the solid-liquid system and avoiding the problem of local overheating to the greatest extent, thereby realizing strict control of the molecular weight distribution and melt index of the polyketone resin, which is also a key factor in the quality assurance of the industrial large-scale production of polyketone resin of the present invention. The equipment cost of the present invention is low and the system control is simple. The slurry from which the monomers are removed after the reaction is fully washed in the slurry washing kettle to remove impurities and elute the catalyst precious metals in the polyketone, and the precious metals in the polyketone resin are fully eluted by controlling the washing temperature, which is beneficial to improving the product purity and precious metal recovery, and the operation cost of the system is low, which is convenient for promotion. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 The present invention is a schematic diagram of a production system of polyketone resin according to an embodiment of the present invention.

[0034] Figure 2 FIG. 1 is a schematic diagram of a production system flow of a polyketone resin according to another embodiment of the present invention.

[0035] Reference numerals:

[0036] 1-reactor; 1a-heat exchanger; 1b-compressor 1; 1c-external circulation pipeline; 2-monomer recovery tank; 2a-gas-liquid separation tank; 2b-compressor 2; 3-slurry washing kettle; 4-solid-liquid separation device; 5-drying device; 6-granulator; 7-solvent recovery tank; 8-solvent distillation tower; 9-precious metal recovery device. DETAILED DESCRIPTION

[0037] The production process and system of the polyketone resin of the present invention are described in detail below.

[0038] The inventors of the present invention have discovered through long-term and multiple experiments that the molecular weight distribution and melt index of polyketone resin are related to the mass transfer and heat transfer conditions during the reaction. By adopting stirring and external circulation in the reaction process to synergistically enhance the mass transfer and heat transfer effects, the quality of polyketone resin is improved. However, the excessive residual palladium in polyketone resin is an important reason for the high cost of polyketone resin. Most of the existing methods for removing residual palladium require complicated processes. The inventors of the present invention unexpectedly discovered that by regulating the washing temperature, the palladium in the polyketone resin can be fully introduced into the washing medium, and the residual palladium in the polyketone resin product can be reduced to below 1 ppm, which greatly reduces the production cost. On this basis, the present invention was completed.

[0039] The first aspect of the present invention provides a production process of a polyketone resin, comprising the following steps:

[0040] Reaction process: adding suspension medium, catalyst, seed and reaction monomer into the reaction device, controlling reaction temperature and reaction pressure, stirring the reaction materials in the reaction device during the reaction, and performing external circulation heat exchange on the reaction materials; the external circulation heat exchange includes continuously leading out the reaction materials in the reaction device, exchanging heat, and then transporting them to below the liquid level of the reaction materials in the reaction device;

[0041] Slurry washing step: washing the slurry containing polyketone with a washing medium to obtain a washed slurry; the washing temperature is 30-80°C;

[0042] Solid-liquid separation step: performing solid-liquid separation on the washed slurry to obtain a solid and a liquid containing a polyketone resin;

[0043] Drying process: Dry the solid containing the polyketone resin to obtain polyketone resin powder or granules.

[0044] In some embodiments of the present invention, the suspension medium in the reaction process is selected from any one or more of methanol, acetone, ethanol, and propanol, preferably methanol.

[0045] In some embodiments of the present invention, the catalyst in the reaction process includes a palladium-containing salt compound, an organic phosphine ligand, a catalyst solvent, and an acid substance; the palladium-containing salt compound includes but is not limited to any one or more of palladium chloride, palladium acetate, palladium sulfate, palladium nitrate, and palladium trifluoroacetate; the organic phosphine ligand includes but is not limited to [(2,2-diethyl-1,3-dioxane-5 ,5-diyl)bis(methylene)]bis[bis(2-methoxyphenyl)phosphine], 1,3-bis(diphenyl-phosphino)propane, 1,3-bis[bis(4-methoxy-phenyl)phosphino]propane, 1,3-bis[bis(2-methoxy-phenyl)phosphino]propane; the catalyst solvent is selected from any one or more of acetone, N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N-methylpyrrolidone (NMP), etc.; the acid substance includes any one or more of sulfuric acid, trifluoroacetic acid, trifluoromethanesulfonic acid, p-toluenesulfonic acid, maleic acid, etc. In some specific embodiments of the present invention, the molar ratio of palladium to the organic phosphine ligand in the palladium-containing salt compound is 1:1-1.5, which can be 1:1-1.1, 1:1.1-1.2, 1:1.2-1.3, 1:1.3-1.4, or 1:1.4-1.5, preferably 1:1-1.2. In some specific embodiments of the present invention, the molar ratio of palladium to the acid substance in the palladium-containing salt compound is 1:5-20, which can be 1:5-10, 1:10-15, or 1:15-20, preferably 1:7-15.

[0046] In some embodiments of the present invention, the seeds in the reaction process are finished powder or granules of polyketone resin.

[0047] In some embodiments of the present invention, the reaction monomers in the reaction process include carbon monoxide, ethylene and / or other olefins; the other olefins are selected from any one or more of propylene, butene, hexene or octene.

[0048] In some embodiments of the present invention, the reaction temperature in the reaction process is 70~95°C, which can be 70~75°C, 75~80°C, 80~85°C, 85~90°C, and can also be 90~95°C; the reaction pressure is 45~60 bar, which can be 45~50 bar, 50~55 bar, and can also be 55~60 bar.

[0049] In some embodiments of the present invention, the reaction time in the reaction step is 4 to 7 h, can be 4 to 5 h, 5 to 6 h, or 6 to 7 h, preferably 6 h.

[0050] In the present invention, the external circulation heat exchange includes continuously extracting the reaction materials in the reaction device, exchanging heat, and then transporting them to below the liquid level of the reaction materials in the reaction device, which can continuously extract the reaction materials located in the center of the reactor, re-introduce them after heat exchange, and cooperate with stirring to enhance the mass transfer and heat transfer effects of the materials in the reactor, greatly avoiding the degradation of the quality of the polyketone resin caused by local overheating. In some embodiments of the present invention, the heat exchange includes heating and / or cooling, and the temperature of the extracted reaction materials is maintained within a specific temperature range by heating or cooling, and the temperature of the reaction materials in the reaction device is controlled by external circulation, thereby effectively controlling the temperature, concentration and reaction rate during the reaction process, improving the uniformity and selectivity of the reaction, and realizing continuous production.

[0051] In some embodiments of the present invention, the temperature of the reaction material after external circulation heat exchange in the reaction process is 50~90°C, and can be 50~55°C, 55~60°C, 60~65°C, 65~70°C, 70~75°C, 75~80°C, 80~85°C, and can also be 85~90°C.

[0052] In some embodiments of the present invention, the washing medium in the slurry washing step is selected from any one or more of methanol, acetone, ethanol, and propanol.

[0053] In some embodiments of the present invention, the washing in the slurry washing process includes stirring washing.

[0054] In some embodiments of the present invention, the washing time in the slurry washing process is 1 to 7 hours, and can be 1 to 2 hours, 2 to 3 hours, 3 to 4 hours, 4 to 5 hours, 5 to 6 hours, or 6 to 7 hours.

[0055] In the present invention, the washing temperature in the slurry washing step is 30-80°C, and can be 30-40°C, 40-50°C, 50-60°C, 60-70°C, or 70-80°C, preferably 50-70°C.

[0056] In the present invention, the solid-liquid separation step and the drying step can be performed separately or simultaneously.

[0057] In some embodiments of the present invention, the solid-liquid separation method in the solid-liquid separation step is selected from centrifugal separation or filtration separation.

[0058] In some embodiments of the present invention, the material temperature of the solid-liquid separation in the solid-liquid separation step is 30-70°C, can be 30-40°C, 40-50°C, 50-60°C, can also be 60-70°C, and more preferably 40-60°C.

[0059] In some embodiments of the present invention, the drying in the drying process is single-stage or multi-stage drying.

[0060] In some embodiments of the present invention, moisture is recovered during the drying process in the drying step.

[0061] In some embodiments of the present invention, the drying in the drying process is single-stage or multi-stage drying.

[0062] In some embodiments of the present invention, the production process further includes one or more of a monomer recovery process, a granulation process, a solvent recovery process, a solvent distillation and purification process, and a precious metal recovery process.

[0063] The monomer recovery process comprises: after the reaction is completed, the material in the reaction device is transported to the monomer recovery device to be separated into a volatile phase containing the monomer and a slurry from which the monomer is removed, and then the volatile phase containing the monomer is subjected to gas-liquid separation, the obtained gas is returned to the reaction device, and the slurry from which the monomer is removed is transported to a slurry washing process.

[0064] In some embodiments of the present invention, the materials in the reaction device in the monomer recovery step are discharged from the bottom of the reactor and transported to the monomer recovery device.

[0065] In some embodiments of the present invention, the temperature in the monomer recovery device in the monomer recovery process is controlled at 30~80°C, which can be 30~35°C, 35~40°C, 40~45°C, 45~50°C, 50~55°C, 55~60°C, 60~65°C, 65~70°C, 70~75°C, and can also be 75~80°C, preferably 50~70°C.

[0066] In some embodiments of the present invention, the liquid obtained by gas-liquid separation in the monomer recovery step is the solvent in the volatile phase and is returned to the monomer recovery device, and the obtained gas is the monomer and is returned to the reaction device.

[0067] In some embodiments of the present invention, the slurry from which monomers are removed in the monomer recovery process is the slurry containing polyketone in the slurry washing process, that is, the slurry from which monomers are removed is discharged from the monomer recovery device and transported to the slurry washing process for washing.

[0068] The granulation process uses the polyketone resin powder or particles obtained in the drying process as raw material, and granulates the polyketone resin particles through a granulation device; in some specific embodiments of the present invention, the granulation process includes mixing the polyketone resin powder or particles with auxiliary materials and then melt granulating them.

[0069] The solvent recovery process recovers the liquid obtained from the solid-liquid separation process and the moisture collected in the drying process, a part of which is reused in the slurry washing process, and the rest is distilled and purified; in some specific embodiments of the present invention, the solvent recovery process includes solvent storage, transfer and recovery, and the recovered solvent includes water, suspension medium, washing medium, oligomers, phosphine ligands in the catalyst, palladium, etc., a part of the recovered solvent is returned to the slurry washing process to maintain the required solvent amount in the slurry washing process, and the rest is transported to the solvent distillation tower for separation and recovery.

[0070] The solvent distillation and purification process separates and purifies the recovered solvent by distilling the recovered solvent to obtain light components, intermediate components and heavy components.

[0071] The precious metal recovery process is to enrich the precious metals in the heavy components obtained after distillation and purification of the recovered solvent in the process to achieve the recovery of precious metals. In some specific embodiments of the present invention, the precious metal recovery process includes filtering and adsorbing the heavy components obtained from the solvent distillation tower to recover the precious metals therein.

[0072] A second aspect of the present invention provides a production system for a polyketone resin, such as Figure 2 As shown, it includes a reaction unit, a slurry washing unit, a centrifugal unit and a drying unit;

[0073] The reaction unit comprises a reactor 1, which is used for reacting to generate a slurry containing polyketone; a stirring assembly for stirring the slurry material is provided inside the reactor 1, an external circulation pipeline 1c communicating with the inside of the reactor 1 is provided outside the reactor 1, and a material outlet of the external circulation pipeline 1c is provided at the lower part of the side wall of the reactor 1, and the homogenization and temperature control of the material in the reactor 1 are achieved through the external circulation pipeline 1c;

[0074] The slurry washing unit comprises a slurry washing kettle 3, which is provided with a slurry inlet containing polyketone and a washing medium adding inlet, and is used to wash the surface of the polyketone and the palladium wrapped inside into the washing medium to obtain a mixed material consisting of the washed slurry and the washing medium;

[0075] The solid-liquid separation unit comprises a solid-liquid separation device 4, the feed inlet of the solid-liquid separation device 4 is connected to the mixed material outlet of the slurry washing kettle 3, and is used for solid-liquid separation of the mixed material to obtain a solid phase containing polyketone and a clear liquid;

[0076] The drying unit comprises a drying device 5 for drying the solid phase containing polyketone to obtain polyketone resin powder or granules.

[0077] In some embodiments of the present invention, Figure 2 As shown, the outer circulation pipeline 1c is provided with a compressor 1b and a heat exchanger 1a in sequence, which are used to perform heat exchange on the material in the outer circulation pipeline 1c, and the material after heat exchange is returned to the reactor 1 through the outer circulation pipeline 1c, so as to achieve homogenization and temperature control of the material in the reactor 1. In some specific embodiments of the present invention, the heat exchanger 1a can be a heat exchanger integrating cooling and heating, or a combination of a refrigerator and a heater.

[0078] In some embodiments of the present invention, a stirring device is provided in the slurry washing kettle 3. In some embodiments of the present invention, a drain valve is provided on the top of the slurry washing kettle 3 to discharge monomers escaped during the slurry washing process.

[0079] In some embodiments of the present invention, the solid-liquid separation device 4 is selected from a centrifuge or a filtering device.

[0080] In some embodiments of the present invention, the drying device 5 is selected from a monopolar drying device or a multi-stage drying device.

[0081] In the present invention, the solid-liquid separation device 4 and the drying device 5 can be separately arranged or integrally arranged. In some embodiments of the present invention, the solid-liquid separation device 4 and the drying device 5 are an integrally arranged filter-drying machine.

[0082] In some embodiments of the present invention, Figure 1 and Figure 2As shown, the production system also includes one or more of a monomer recovery unit, a granulation unit, a solvent recovery unit, a solvent distillation and purification unit, and a precious metal recovery unit.

[0083] In some embodiments of the present invention, the monomer recovery unit includes a monomer recovery tank 2, which is provided with a material inlet and a volatile phase outlet containing monomers at the top, a liquid phase inlet at the side, and a slurry outlet for removing monomers at the bottom; the material inlet is connected to the material outlet at the bottom of the reactor 1, so that the material obtained by the reaction enters the monomer recovery tank 2 and is separated into a volatile phase containing monomers and a slurry for removing monomers; the outside of the monomer recovery tank 2 is provided with a gas-liquid separation device connected to the inside of the monomer recovery tank 2, which is used to perform gas-liquid separation on the volatile phase containing monomers. In some specific embodiments of the present invention, the monomer recovery tank 2 is located at the lower position of the reactor. After the reaction is completed, the material in the reactor 1 is discharged from the material outlet at the bottom of the reactor 1 and enters the monomer recovery tank 2 under the action of pressure difference and gravity. In other specific embodiments of the present invention, a delivery pump is provided on the connecting pipeline between the material outlet at the bottom of the reactor 1 and the material inlet at the top of the monomer recovery tank 2, and the delivery pump is selected from a mixed flow pump or a centrifugal pump. In some embodiments of the present invention, Figure 2 As shown, the gas-liquid separation device includes a gas-liquid separation tank 2a, and the gas-liquid separation tank 2a is provided with a volatile phase inlet containing monomers, a liquid phase outlet and a gas phase outlet. The volatile phase inlet containing monomers is connected to the volatile phase outlet containing monomers of the monomer recovery tank 2, the liquid phase outlet is connected to the liquid phase inlet of the monomer recovery tank 2, the gas phase outlet is connected to the material inlet of the reactor 1, and a compressor 2b and a heat exchanger 2 are provided on the connecting pipeline between the gas phase outlet and the material inlet of the reactor 1, so as to realize the recovery of monomers. In some specific embodiments of the present invention, as Figure 1 As shown, the connecting pipeline between the gas phase outlet and the material inlet of the reactor 1 is parallel to the external circulation pipeline 1c downstream of the compressor 2b to share a heat exchanger, that is, the heat exchanger 1a also serves as the heat exchanger 2.

[0084] In some embodiments of the present invention, the granulation unit comprises a granulator 6 for preparing polyketone resin granules from the polyketone resin powder or granules obtained in the drying process.

[0085] In some embodiments of the present invention, the solvent recovery unit includes a solvent recovery tank 7, the inlet of the solvent recovery tank 7 is respectively connected to the liquid outlet of the solid-liquid separation device 4 and the solvent outlet of the drying device 5, and the solvent recovery tank 7 is provided with two outlets, one outlet is connected to the washing medium inlet of the slurry washing kettle 3, and the other outlet is connected to the feed port of the solvent distillation device in the system.

[0086] In some embodiments of the present invention, the solvent distillation and purification unit comprises a solvent distillation tower 8, the feed port of the solvent distillation tower 8 is connected to the outlet of the solvent recovery device in the system, and is used to distill the recovered solvent. The top of the tower is provided with a light component outlet, the bottom of the tower is provided with a heavy component outlet, and the middle of the tower is provided with an intermediate component outlet. In some embodiments of the present invention, the solvent distillation tower 8 is a plate tower or a packed tower; preferably a plate tower, the theoretical number of plates is 5 to 45, the reflux ratio is 0.5 to 5, the light component is extracted from the top of the tower, the heavy component is discharged from the bottom of the tower, and the intermediate component is extracted through the side line.

[0087] In some embodiments of the present invention, the precious metal recovery unit includes a precious metal recovery device 9, which is used to enrich the precious metals in the heavy components obtained after distillation and purification of the recovered solvent. In some embodiments of the present invention, the precious metal recovery device 9 includes a filter and an adsorption device, which are used to intercept the precious metals in the recovered solvent and the washing medium. Preferably, the filter is selected from a filter element filter, made of stainless steel, with a pore size of 1 to 10 microns; preferably, the adsorption material of the adsorption device is selected from activated carbon or an ion exchange resin that selectively adsorbs the precious metals in the catalyst.

[0088] The technical solution of the present invention is described below through specific examples. It should be understood that the one or more method steps mentioned in the present invention do not exclude the existence of other method steps before and after the combination step or the insertion of other method steps between these explicitly mentioned steps; it should also be understood that these embodiments are only used to illustrate the present invention and are not used to limit the scope of the present invention. Moreover, unless otherwise specified, the numbering of each method step is only a convenient tool for identifying each method step, and is not intended to limit the order of arrangement of each method step or to limit the scope of the present invention. The change or adjustment of the relative relationship thereof shall also be regarded as the scope of the present invention without substantially changing the technical content.

[0089] The molecular weight distribution test method is as follows:

[0090] Hexafluoroisopropanol was used as solvent, and the polymer was prepared to 0.001 g / mL; hexafluoroisopropanol (containing 0.1 mM trifluoroacetic acid) was used as mobile phase; the column was Shodex HFIP-806M model, the detector was RI detector, and the temperature was 35 °C;

[0091] The melt index test method is as follows:

[0092] Refer to "Standard Test Method for Melt Flow Rate of Thermoplastics Using Extrusion Rheometer" (ASTM D1238). Temperature 240 ℃, weight pressure 2.16 kg.

[0093] Example 1

[0094] The production system of the polyketone resin in this embodiment is as follows Figure 1 As shown, the following steps are included:

[0095] S1. Preparation of catalyst: Dissolve 4 g (0.018 mol) of palladium acetate in 3.8 liters of acetone, add 13.11 g (0.02 mol) of bidentate organophosphine ligand [(2,2-diethyl-1,3-dioxane-5,5-diyl)bis(methylene)]bis[bis(2-methoxyphenyl)phosphine], stir and dissolve at 25 °C, add 14.25 ml (0.19 mol) of trifluoroacetic acid, stir for 1 h to obtain the catalyst, which is ready for use.

[0096] S2, reaction process: add 700 liters of methanol and 3.8 liters of catalyst into a 1000 liter reactor 1, and add 15.4 kg of polyketone finished product as seeds, replace the gas in the reactor 1 with nitrogen for 5 times, and then pump in 48 kg of propylene; heat the reactor 1 to 70 ° C, and then introduce a mixture of carbon monoxide and ethylene (molar ratio 1:1) to make the pressure in the reactor 1 reach 50 bar, and the reaction lasts for 6 hours to generate a slurry containing polyketone; during the reaction, turn on the stirring component in the reactor 1 to mechanically stir the material; at the same time, turn on the external circulation function of the reactor 1 to perform external circulation heat exchange on the material in the reactor 1 to maintain the material temperature at 65 o C, thereby achieving homogenization and temperature control of the materials in the reactor 1.

[0097] S3, slurry washing process: after the reaction is carried out for 6 hours, the reaction is terminated by lowering the temperature in the reactor 1 and releasing the pressure. After the temperature in the reactor 1 is lowered to 50°C and the pressure is lowered to 3 bar, the material outlet valve at the bottom of the reactor 1 is opened, and the material in the reactor is transferred to the slurry washing reactor 3 by the pressure difference and the height difference. The temperature in the slurry washing reactor 3 is adjusted to maintain at 50°C, the stirring device in the slurry washing reactor 3 is turned on, and the washing medium is introduced through the washing medium inlet of the slurry washing reactor 3 at the same time, and stirred. The escaping monomer is discharged through the drain valve on the top of the slurry washing reactor 3. After stirring and washing for 6 hours, the surface of the polyketone and the palladium wrapped inside are washed into the washing medium to obtain a mixed material consisting of the washed slurry and the washing medium.

[0098] S4, solid-liquid separation process and drying process: conveying the mixed material consisting of the washed slurry and the washing medium to a filter-dryer integrated machine, and maintaining the temperature of the filter-dryer integrated machine (the filter-dryer integrated machine also serves as the solid-liquid separation device 4 and the drying device 5) at 50° C. to obtain a polyketone resin powder;

[0099] S5, solvent recovery process: the methanol filtrate obtained by the filter-dryer is collected and transported to the solvent recovery tank 7 for recycling.

[0100] 174.3 kg of polyketone resin powder was collected. The melt index of the polyketone resin product was 4.6 g / 10 min and the molecular weight distribution was 2.2. The catalytic efficiency was 83.6 kg polyketone / g palladium. The residual palladium in the product was 0.93 ppm.

[0101] Example 2

[0102] The production system of the polyketone resin in this embodiment is as follows Figure 2 As shown, the following steps are included:

[0103] S1. Preparation of catalyst: Dissolve 0.28 kg (1.26 mol) of palladium acetate in 266 L of acetone, add 918 g (1.4 mol) of bidentate organophosphine ligand [(2,2-diethyl-1,3-dioxane-5,5-diyl)bis(methylene)]bis[bis(2-methoxyphenyl)phosphine], stir and dissolve at 25 °C, add 1.0 L (13.3 mol) of trifluoroacetic acid, stir for 1 h to obtain the catalyst, and set aside.

[0104] S2, reaction process: to 80 m 3 Add 49 m 3 Methanol and 266 liters of catalyst, and 1080 kg of polyketone finished product was added as seeds, the gas in reactor 1 was replaced 5 times with nitrogen, and then 3.36 t of propylene was pumped in; the reactor 1 was heated to 70 ° C, and then a mixture of carbon monoxide and ethylene (molar ratio 1:1) was introduced to make the pressure in reactor 1 reach 50 bar, the reaction lasted for 6 hours, and the reaction generated a slurry containing polyketone; during the reaction, the stirring component in reactor 1 was turned on to mechanically stir the material; at the same time, the material in reactor 1 entered the external circulation pipeline 1c, and heat was exchanged with the material in the external circulation pipeline 1c through the heat exchanger 1a to maintain the material temperature at 65 o C, and then returns to the reactor 1, thereby achieving homogenization and temperature control of the materials in the reactor 1.

[0105] S3, monomer recovery process: after the reaction is carried out for 6 hours, the reaction is terminated by lowering the temperature in the reactor 1 and releasing the pressure. After the temperature in the reactor 1 is lowered to 50°C and the pressure is lowered to 3 bar, the material outlet valve at the bottom of the reactor 1 is opened. Since the monomer recovery tank 2 is located below the reactor 1, the slurry containing polyketone in the reactor 1 enters the monomer recovery tank 2 under the action of pressure difference and height difference, and is separated into a volatile phase containing monomer and a slurry from which the monomer is removed. The volatile phase containing monomer (i.e., the monomer that has not reacted completely and entrains the solvent) enters the gas-liquid separation tank 2a through a pipeline from the volatile phase outlet containing monomer at the top of the monomer recovery tank 2, is cooled in the gas-liquid separation tank 2a, and gas-liquid separation occurs. After cooling, the solvent becomes a liquid phase and returns to the monomer recovery tank 2. The non-condensable monomer is discharged through the gas phase outlet at the top of the gas-liquid separation tank 2a, is compressed by a compressor 2b, and then passes through a heat exchanger 1a. The compressed non-condensable monomer is heat-exchanged by the heat exchanger 1a to maintain its temperature at 65 o C, and then returned to the reactor 1.

[0106] S4, slurry washing process: adjust the temperature in the slurry washing kettle 3 to maintain it at 50°C, transfer the slurry from which the monomers are removed in the monomer recovery tank 2 to the slurry washing kettle 3, turn on the stirring device in the slurry washing kettle 3, and simultaneously introduce the washing medium through the washing medium inlet of the slurry washing kettle 3, stir, and the escaping monomer is discharged through the drain valve on the top of the slurry washing kettle 3. After stirring and washing for 6 hours, the surface of the polyketone and the palladium wrapped inside are washed into the washing medium to obtain a mixed material consisting of the washed slurry and the washing medium.

[0107] S5, solid-liquid separation (centrifugation) step: the mixed material consisting of the washed slurry and the washing medium is transported to the solid-liquid separation device (centrifuge) 4 for centrifugal separation to obtain a solid phase containing polyketone and a clear liquid.

[0108] S6, drying process: the solid phase containing polyketone is transferred to the drying device 4 (multi-stage drying device), and the temperature of the drying device 4 is maintained at 50° C. to obtain polyketone resin powder.

[0109] S7, solvent recovery process: the clear liquid and the wet part collected by the filter-dryer are transported to the solvent recovery tank 7 together, the first outlet of the solvent recovery tank 7 is connected to the washing medium inlet of the slurry washing kettle 3, and a part of the recovered solvent is reused in the slurry washing process. The solvent recovery tank 7 is also provided with a second outlet.

[0110] S8, solvent distillation and purification process: the remaining part of the recovered solvent is transported to the solvent distillation tower 8 through the second outlet, and the recovered solvent is distilled and purified. The theoretical number of plates is 25, the reflux ratio is 0.5-5, the light components are extracted from the top of the tower, the heavy components are discharged from the bottom of the tower, and the intermediate components are extracted through the side line.

[0111] S9, precious metal recovery process: the heavy components at the bottom of the solvent distillation tower 8 are transported to the precious metal recovery device 9, and the precious metals are enriched and recovered through the filter and the adsorption device.

[0112] 1.23 t of polyketone resin powder was obtained, the melt index of the polyketone resin product was 4.4 g / 10 min, the molecular weight distribution was 2.1, the catalytic efficiency was 85.1 kg polyketone / g palladium, and the residual palladium in the product was 0.88 ppm.

[0113] Example 3

[0114] Except that the reaction kettle temperature in step S2 is controlled to be 80° C. and the reaction time is 5 hours, the rest is the same as in Example 1.

[0115] Example 4

[0116] Except that the reaction kettle temperature in step S2 is controlled to be 95° C. and the reaction time is 4 hours, the rest is the same as in Example 1.

[0117] Example 5

[0118] Except that the reaction time was 7 hours, the rest was the same as in Example 1.

[0119] Example 6

[0120] Except that the molar ratio of the organophosphorus ligand to palladium acetate in the preparation of the catalyst in step S1 is controlled to be 1.21:1, the rest is the same as in Example 1.

[0121] Example 7

[0122] Except that the molar ratio of the organophosphorus ligand to palladium acetate in the preparation of the catalyst in step S1 is controlled to be 1.05:1, the rest is the same as in Example 1.

[0123] Example 8

[0124] Except that the molar ratio of trifluoroacetic acid to palladium acetate in the preparation of the catalyst in step S1 is controlled to be 5.5:1, the rest is the same as in Example 1.

[0125] Example 9

[0126] Except that the molar ratio of trifluoroacetic acid to palladium acetate in the preparation of the catalyst in step S1 is controlled to be 11.5:1, the rest is the same as in Example 1.

[0127] Example 10

[0128] Except that the pressure in the reactor is controlled to be 45 bar in the reaction process of step S2, the rest is the same as in Example 1.

[0129] Embodiment 11

[0130] Except that the pressure in the reactor is controlled to be 60 bar in the reaction process of step S2, the rest is the same as in Example 1.

[0131] Example 12

[0132] Except that the temperature of the slurry washing kettle in step S4 is controlled to be 30°C, the rest is the same as in Example 1.

[0133] Embodiment 13

[0134] Except that the temperature of the slurry washing kettle in step S4 is controlled to be 80°C, the rest is the same as in Example 1.

[0135] Comparative Example 1

[0136] Except that no external circulation heat exchange is performed in the reaction process of step S2, the rest is the same as in Example 1.

[0137] Comparative Example 2

[0138] Except that the temperature of the slurry washing kettle in step S4 is controlled to be 20°C, the rest is the same as in Example 1.

[0139] Comparative Example 3

[0140] Except that the temperature of the slurry washing kettle in step S4 is controlled to be 90°C, the rest is the same as in Example 1.

[0141] The performance analysis of the polyketone resin samples prepared in Examples 1 to 13 and Comparative Examples 1 to 3 is shown in Table 1 below.

[0142] Table 1 Performance analysis of polyketone resin samples prepared in Examples 1 to 13 and Comparative Examples 1 to 3

[0143]

[0144] As can be seen from Table 1, by comparing the performance of the polyketone resin samples prepared in Example 1 and Comparative Example 1, it can be seen that Comparative Example 1 did not perform external circulation heat exchange, the heat exchange efficiency was low, the temperature in the kettle was uneven, the catalytic efficiency remained unchanged, the product molecular weight distribution increased, and the melt index increased, indicating that external circulation heat exchange plays a key role in improving the quality of polyketone.

[0145] By comparing the performance of the polyketone resin samples prepared in Example 1 and Examples 3-4, it can be seen that as the reaction temperature increases, the melt index of the polyketone resin increases, which means that the molecular weight decreases. The molecular weight distribution decreases as the melt index increases.

[0146] By comparing the performance of the polyketone resin samples prepared in Example 1 and Examples 6-7, it can be seen that changing the reaction time and the amount of phosphine ligand within a certain range will not significantly affect the polymerization results. However, there is an optimal amount of phosphine ligand, and too high or too low an amount will reduce the efficiency of polymerization. Too low an amount of phosphine ligand will also result in more palladium residues in the final product.

[0147] By comparing the performance of the polyketone resin samples prepared in Example 1 with those prepared in Examples 8-9, it can be seen that too low a dosage of trifluoroacetic acid not only reduces the polymerization efficiency, but also results in more palladium residues in the final product.

[0148] By comparing the performance of the polyketone resin samples prepared in Example 1 with those prepared in Examples 10-11, it can be seen that too low a reaction pressure reduces the polymerization efficiency.

[0149] By comparing the performance of the polyketone resin samples prepared by Example 1 with Examples 12-13 and Comparative Examples 2-3, it can be seen that the washing temperature has a great influence on the catalytic efficiency and the palladium residue on the product. The palladium residue in the product of Comparative Example 2 is significantly higher than that in Example 12, indicating that the palladium residue increases as the washing temperature decreases. Therefore, moderately increasing the washing temperature is beneficial to washing out the residual palladium from the polyketone product. The possible reasons are that heating is beneficial to the dissociation of the palladium complex or the liberation of palladium ions, and secondly, the polyketone solid will have a more obvious swelling after heating, which is beneficial to the opening of the pores in the polyketone particle structure and the release of the encapsulated residual palladium. The palladium residue in the products of Example 12 and Comparative Example 3 is close to that of Example 12, indicating that after the temperature reaches 70°C, the effect of continuing to heat up for the recovery of precious metals is no longer obvious. Too high a temperature will have more waste in energy consumption, and it will also require the material to undergo an additional cooling before it can be connected with the subsequent processing steps, resulting in a more complicated process.

[0150] The above embodiments are merely illustrative of the principles and effects of the present invention, and are not intended to limit the present invention. Anyone familiar with the art may modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by a person of ordinary skill in the art without departing from the spirit and technical concept disclosed by the present invention shall still be covered by the claims of the present invention.

Claims

1. A production process for a polyketone resin, characterized in that: Including the following processes: Reaction process: adding suspension medium, catalyst, seed and reaction monomer into the reaction device, controlling the reaction temperature to be 70-95°C, the reaction pressure to be 45-60 bar, stirring the reaction materials in the reaction device during the reaction, and performing external circulation heat exchange on the reaction materials; the external circulation heat exchange includes continuously leading out the reaction materials in the reaction device, exchanging heat, and then transporting them to below the liquid level of the reaction materials in the reaction device; the temperature of the reaction materials after external circulation heat exchange is 50-90°C; Slurry washing step: washing the slurry containing polyketone with a washing medium to obtain washed slurry; The washing temperature is 30-80°C; Solid-liquid separation step: performing solid-liquid separation on the washed slurry to obtain a solid and a liquid containing a polyketone resin; Drying process: drying the solid containing polyketone resin to obtain polyketone resin powder or granules; It also includes one or more of a monomer recovery process, a granulation process, a solvent recovery process, a solvent distillation and purification process, and a precious metal recovery process; The monomer recovery process comprises: after the reaction is completed, the material in the reaction device is transported to the monomer recovery device, and is separated into a volatile phase containing the monomer and a slurry from which the monomer is removed, and then the volatile phase containing the monomer is subjected to gas-liquid separation, the obtained gas is returned to the reaction device, and the slurry from which the monomer is removed is transported to a slurry washing process; The granulation process uses the polyketone resin powder or particles obtained in the drying process as raw materials, and granulates them through a granulation device to obtain polyketone resin particles; The solvent recovery step recovers the liquid obtained in the solid-liquid separation step and the moisture collected in the drying step, a part of which is reused in the slurry washing step, and the rest is distilled and purified; The solvent distillation and purification process separates and purifies the recovered solvent by distilling the recovered solvent to obtain light components, intermediate components and heavy components; The precious metal recovery step is to enrich the precious metals in the heavy components obtained after the recovery solvent is distilled and purified in the process, so as to achieve the recovery of precious metals.

2. The production process of the polyketone resin according to claim 1, characterized in that: The reaction process includes one or more of the following features: (a) the suspension medium is selected from any one or more of methanol, acetone, ethanol and propanol; (b) the catalyst comprises a palladium-containing salt compound, an organic phosphine ligand, a catalyst solvent, and an acid substance; (c) the seeds are finished powder or granules of polyketone resin; (d) the reactive monomers include carbon monoxide, ethylene and / or other olefins; (e) The reaction time is 4 to 7 h.

3. The production process of the polyketone resin according to claim 2, characterized in that: Includes one or more of the following characteristics: b1) The palladium-containing salt compound includes any one or more of palladium chloride, palladium acetate, palladium sulfate, palladium nitrate, and palladium trifluoroacetate; b2) The organic phosphine ligands include [(2,2-diethyl-1,3-dioxane-5,5-diyl)bis(methylene)]bis[bis(2-methoxyphenyl)phosphine], 1,3-bis(diphenyl-phosphino)propane, 1,3-bis[bis(4-methoxy-phenyl)phosphino]propane, 1,3-bis[bis(2-methoxy-phenyl)phosphino]propane; b3) the catalyst solvent is selected from any one or more of acetone, N,N-dimethylformamide, dimethyl sulfoxide, and N-methylpyrrolidone; b4) The acid substance includes any one or more of sulfuric acid, trifluoroacetic acid, trifluoromethanesulfonic acid, p-toluenesulfonic acid, and maleic acid; b5) the molar ratio of the palladium-containing salt compound to the organic phosphine ligand is 1:1 to 1.5; b6) the molar ratio of the palladium-containing salt compound to the acid substance is 1:5-20; b7) The other olefins are selected from any one or more of propylene, butene, hexene or octene.

4. The production process of the polyketone resin according to claim 1, characterized in that: Includes one or more of the following characteristics: 1) In the slurry washing step, the washing medium is selected from any one or more of methanol, acetone, ethanol, and propanol; 2) In the slurry washing process, the washing includes stirring washing; 3) In the slurry washing process, the washing time is 1 to 7 hours; 4) In the solid-liquid separation step, the solid-liquid separation method is selected from centrifugal separation or filtration separation; 5) In the solid-liquid separation process, the temperature of the solid-liquid separation material is 30~70℃; 6) In the drying process, the drying is single-stage or multi-stage drying; 7) In the drying process, the moisture is recovered during the drying process.

5. The production process of the polyketone resin according to claim 1, characterized in that: The monomer recovery process includes one or more of the following features: i) the materials in the reaction device are discharged from the bottom of the reactor and transported to the monomer recovery device; ii) the temperature in the monomer recovery device is controlled at 30-80°C; iii) the liquid obtained from the gas-liquid separation is returned to the monomer recovery device, and the gas obtained is returned to the reaction device; iv) The slurry from which the monomers are removed is the slurry containing polyketone in the slurry washing step.

6. A polyketone resin production system used in the polyketone resin production process according to claim 1, characterized in that: It includes a reaction unit, a slurry washing unit, a solid-liquid separation unit and a drying unit; The reaction unit comprises a reactor for reacting to generate a slurry containing polyketone; a stirring assembly for stirring the slurry material is arranged inside the reactor, an external circulation pipeline communicating with the inside of the reactor is arranged outside the reactor, a material outlet of the external circulation pipeline is arranged at the lower part of the side wall of the reactor, and the homogenization and temperature control of the material in the reactor are achieved through the external circulation pipeline; The slurry washing unit comprises a slurry washing kettle, which is provided with a slurry inlet containing polyketone and a washing medium adding inlet, and is used to wash the surface of the polyketone and the palladium wrapped inside into the washing medium to obtain a mixed material consisting of the washed slurry and the washing medium; The solid-liquid separation unit comprises a solid-liquid separation device, the feed inlet of the solid-liquid separation device is connected to the mixed material outlet of the slurry washing kettle, and is used for solid-liquid separation of the mixed material to obtain a solid phase containing polyketone and a clear liquid; The drying unit includes a drying device for drying the solid phase containing polyketone to obtain polyketone resin powder or granules; It also includes one or more of a monomer recovery unit, a granulation unit, a solvent recovery unit, a solvent distillation and purification unit, and a precious metal recovery unit; The monomer recovery unit comprises a monomer recovery tank, wherein the top of the monomer recovery tank is provided with a material inlet and a volatile phase outlet containing monomers, the side is provided with a liquid phase inlet, and the bottom is provided with a slurry outlet for removing monomers; the material inlet is connected with the material outlet at the bottom of the reactor, so that the material obtained by the reaction enters the monomer recovery tank and is separated into a volatile phase containing monomers and a slurry for removing monomers; the outside of the monomer recovery tank is provided with a gas-liquid separation device connected with the inside of the monomer recovery tank, which is used for gas-liquid separation of the volatile phase containing monomers; The granulation unit includes a granulator for preparing polyketone resin particles from the polyketone resin powder or particles obtained in the drying process; The solvent recovery unit comprises a solvent recovery tank, the inlet of the solvent recovery tank is respectively connected to the liquid outlet of the solid-liquid separation device and the solvent outlet of the drying device, and the solvent recovery tank is provided with two outlets, one outlet is connected to the washing medium inlet of the slurry washing kettle, and the other outlet is connected to the feed inlet of the solvent distillation device in the system; The solvent distillation and purification unit comprises a solvent distillation tower, the feed port of which is connected to the outlet of the solvent recovery device in the system, and is used to distill the recovered solvent, the tower top is provided with a light component outlet, the tower bottom is provided with a heavy component outlet, and the middle of the tower is provided with an intermediate component outlet; The precious metal recovery unit comprises a precious metal recovery device, which is used for enriching and recovering precious metals in the heavy components obtained after distillation and purification of the solvent.

7. The polyketone resin production system according to claim 6, characterized in that: Includes one or more of the following characteristics: (1) A compressor 1 and a heat exchanger 1 are sequentially arranged on the external circulation pipeline for exchanging heat with the material in the external circulation pipeline; (2) A stirring device is provided in the slurry washing kettle; (3) A drain valve is provided on the top of the slurry washing kettle; (4) The solid-liquid separation device is selected from a centrifuge or a filtering device; (5) The drying device is selected from a single-stage drying device or a multi-stage drying device.

8. The polyketone resin production system according to claim 6, characterized in that: Includes one or more of the following characteristics: a) the gas-liquid separation device comprises a gas-liquid separation tank, the gas-liquid separation tank is provided with a volatile phase inlet containing monomers, a liquid phase outlet and a gas phase outlet, the volatile phase inlet containing monomers is communicated with the volatile phase outlet containing monomers of the monomer recovery tank, the liquid phase outlet is communicated with the liquid phase inlet of the monomer recovery tank, the gas phase outlet is communicated with the material inlet of the reactor, and a second compressor and a second heat exchanger are provided on the communication pipeline between the gas phase outlet and the material inlet of the reactor, so as to realize the recovery of monomers; b) the solvent distillation tower is a plate tower or a packed tower; c) the precious metal recovery unit is used to recover the precious metals in the heavy components obtained from the solvent distillation tower; d) The precious metal recovery device includes a filter and an adsorption device.

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