Production method of poly (co-itaconic acid)

By introducing the polymerized dry material directly into the chip machine and utilizing the functions of washing and cooling media, combined with the design of anchor stirring paddles and insulation pipes, the problems of complicated operation and low efficiency in the existing technology are solved, and high efficiency and low efficiency are achieved Cost of co-production.

CN119191930AInactive Publication Date: 2024-12-27浙江材华科技有限公司

Patent Information

Application Number
CN202411699505.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-26
Publication Date
2024-12-27
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

The existing co-uncil production process is complicated to operate, has high cost and low production efficiency, and requires simplification of the process to improve efficiency and reduce costs.

Method used

The reaction-derived polylinked material is directly introduced into the pellet machine, and adhered to the surface of the drum through the action of washing medium and cooling medium to avoid stirring and precipitation and filtration steps. The temperature is controlled by an anchor stirring paddle and jacket. Set up insulation pipes to reduce product losses.

Benefits of technology

The operation process is simplified, production efficiency is improved, product yield and purity is improved, construction and operation costs are reduced, and continuous preparation of gangs is realized.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a production method of polymersome, and belongs to the technical field of polymersome production. The method comprises the following steps: directly introducing a poly-linked material obtained by reacting di-tert-butyl peroxide and diisopropylbenzene in a reaction kettle into a flaker comprising an immersion tank, a rotary drum and a scraper system; washing the poly-coupled wilt material introduced into the leaching tank by using a washing medium; a cooling medium is sprayed towards the rotary drum through a spraying system, so that the washed materials are attached to the surface of the rotary drum based on the cooling effect of the cooling medium in the rotating process of the rotary drum; and the scraper system is used for scraping off the poly-mercuric chloride product attached to the surface of the rotary drum. According to the present invention, the poly-union-cake material obtained through the reaction is directly introduced into the flaker, such that the stirring precipitation process is avoided, and the step of separation through the plate-and-frame filter press or the centrifuge after the poly-union-cake material is subjected to stirring precipitation in the stirring kettle in the prior art is omitted, such that the operation is reduced, the efficiency is easily improved, the cost is easily saved, and the product yield and the product purity are high.
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Description

Technical Field

[0001] The present invention relates to the technical field of poly-copper production, and in particular to a method for producing poly-copper. Background Art

[0002] Diisopropylbenzene oligomers, also known as poly(diisopropylbenzene), are oxygen-free carbon-based free radical initiators with a special structure that is highly aggregated. They are considered to be an important functional molecule with multiple biological activities and application prospects.

[0003] At present, the production process of polylinker is to heat up the reactor through a heat exchanger, add di-tert-butyl peroxide (DTBP) in a high-level tank, react in the reactor, and connect a condensation device above the reactor. For the bottom of the reactor, the material is introduced into the stirring tank with insulation, stirred and precipitated, and then generally a plate and frame filter press or a centrifuge is used to filter and discard the material, and the product is packaged. The above operation is relatively complicated, costly, and has low production efficiency.

[0004] In view of this, the present invention is proposed. Summary of the invention

[0005] The object of the present invention is to provide a method for producing polyunsaturated fat to solve or improve the above-mentioned technical problems.

[0006] The present invention can be implemented like this: In a first aspect, the present invention provides a method for producing poly-copper nitrate, comprising the following steps: directly introducing the poly-copper nitrate material obtained by reacting di-tert-butyl peroxide and diisopropylbenzene in a reactor into a flaker including an immersion tank, a rotary drum and a scraper system; The poly-drying material introduced into the immersion tank is washed by the washing medium; the cooling medium is sprayed toward the drum by the spray system, so that the washed material adheres to the surface of the drum due to the cooling effect of the cooling medium during the rotation of the drum; the poly-drying product adhering to the surface of the drum is scraped off by the scraper system.

[0007] In an optional embodiment, the reaction of di-tert-butyl peroxide and diisopropylbenzene in a reactor includes: adding di-tert-butyl peroxide to diisopropylbenzene at a temperature of 130° C. to 135° C. in the reactor at a molar ratio of diisopropylbenzene to di-tert-butyl peroxide of 1:1 to 1:2, until the content of di-tert-butyl peroxide in the reaction solution does not exceed 5wt%, and then stopping the reaction.

[0008] In an optional embodiment, the introduction rate of di-tert-butyl peroxide is 400 mL / s to 400 mL / 2s.

[0009] In an alternative embodiment, the actual reaction temperature of the reaction process does not exceed 125°C.

[0010] In an optional embodiment, an anchor-type stirring paddle is provided in the reactor.

[0011] In an alternative embodiment, the reactor has a jacket.

[0012] In an optional embodiment, a shell and tube heat exchanger is connected to the top of the reactor to perform heat exchange and recovery on the gas evaporated from the top of the reactor.

[0013] In an optional embodiment, the reactor and the flaker are connected by a pipeline, and the outer wall of the pipeline has a heat-insulating structure.

[0014] In an optional embodiment, the temperature of the cooling medium is 12°C to 18°C.

[0015] In an optional embodiment, 1.6 m 3 For the polymerized dry materials, the speed of the drum is 3r / min~5r / min.

[0016] The beneficial effects of the present invention include: The present invention directly introduces the poly-coke material obtained by the reaction into a flaker, thereby avoiding the stirring and settling process, eliminating the steps in the prior art in which the poly-coke material needs to be stirred and precipitated in a stirring kettle and then separated by a plate and frame filter press or a centrifuge, reducing operations, being conducive to improving efficiency and saving costs, and having high product yield and purity. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for use in the embodiments are briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without creative work.

[0018] Figure 1 This is a production system structure diagram of the production method of the poly-linked dry product provided by the present invention.

[0019] Icons: 10-reactor; 11-first inlet; 12-second inlet; 20-flaking machine; 30-high-level tank; 40-shell and tube heat exchanger; 50-recovery tank; 61-diisopropylbenzene storage container; 62-di-tert-butyl peroxide storage container; 63-washing agent storage container. DETAILED DESCRIPTION

[0020] In order to make the purpose, technical scheme and advantages of the embodiments of the present invention clearer, the technical scheme in the embodiments of the present invention will be described clearly and completely below. If the specific conditions are not specified in the embodiments, they are carried out according to conventional conditions or conditions recommended by the manufacturer. If the manufacturer of the reagents or instruments used is not specified, they are all conventional products that can be purchased commercially.

[0021] The production method of the poly-linked carbon provided by the present invention is specifically described below.

[0022] Please refer to Figure 1 The production of the polyunsaturated fat provided by the present invention is carried out in a specific production system.

[0023] The production system includes a polymerization unit and a post-processing unit.

[0024] The polymerization unit includes a reactor 10, and the post-processing unit includes a flaker 20 and a spraying system (not shown).

[0025] The top of the reactor 10 has an inlet for introducing the reaction materials. In some embodiments, it can be divided into a first inlet 11 for introducing diisopropylbenzene and a second inlet 12 for introducing di-tert-butyl peroxide. In other embodiments, diisopropylbenzene and di-tert-butyl peroxide can be introduced through the same inlet.

[0026] The raw material di-tert-butyl peroxide can be pre-stored in a di-tert-butyl peroxide storage container 62 (such as a container in the form of a storage tank or a storage tank), and the di-tert-butyl peroxide storage container 62 is connected to the inlet for introducing di-tert-butyl peroxide of the reactor 10 through a pipeline. In some embodiments, an overhead tank 30 is further provided between the di-tert-butyl peroxide storage container 62 and the inlet for introducing di-tert-butyl peroxide of the reactor 10.

[0027] The raw material diisopropylbenzene may be pre-stored in a diisopropylbenzene storage container 61 (such as a container in the form of a storage tank or a storage tank), and the diisopropylbenzene storage container 61 is connected to the inlet of the reactor 10 for introducing diisopropylbenzene through a pipeline.

[0028] The top of the reactor 10 is connected to a condensation recovery system to recover the gas evaporated from the top of the reactor, and the condensation recovery system includes a shell and tube heat exchanger 40 and a recovery tank 50. The cold fluid flows through the shell side, and the hot fluid flows through the tube side, and then the evaporated gas is recovered after heat exchange.

[0029] The bottom of the reactor 10 is connected to the flaker 20 through a pipeline. The flaker 20 includes an immersion tank (not shown), a rotary drum (not shown) and a scraper system (not shown). The bottom of the reactor 10 is connected to the immersion tank of the flaker 20 through a pipeline to directly introduce the reaction product obtained in the reactor 10 into the immersion tank of the flaker 20. The nozzle of the spray system is directed toward the rotary drum to spray the cooling medium (such as cooling water) on the rotary drum, so that the material brought out during the rotation of the rotary drum forms a solid under the cooling effect of the cooling medium and adheres to the surface of the rotary drum. The scraper system is used to scrape the solid material attached to the surface of the rotary drum and drop it into the material tray (not shown) of the flaker 20.

[0030] In some embodiments, the surface of the drum is provided with spiral grooves to facilitate the operation of the scraper.

[0031] In addition, the immersion tank of the flaker 20 is also connected to a washing agent storage container 63 for storing a washing agent. The washing agent may be, for example, ethanol. By introducing ethanol into the immersion tank, the reaction product introduced into the immersion tank is washed.

[0032] In some embodiments, an anchor-type stirring paddle is provided in the reactor 10. Furthermore, the reactor 10 also has a jacket.

[0033] It should be noted that, in the reactor 10, after the reaction of diisopropylbenzene and di-tert-butyl peroxide, the transfer coefficient will decay in the reactor 10, which makes the temperature control in the reactor 10 inaccurate, and the product yield is very sensitive to the stability of the total heat input of the reactor 10, resulting in a significant loss of product yield. By arranging an anchor-type stirring paddle in the reactor 10, the surface heat transfer coefficient can be maximized. The reactor 10 has a jacket, and steam is introduced into the jacket, so that the temperature can be controlled by controlling the steam flow rate, and the product yield is improved.

[0034] The reaction kettle 10 and the flaker 20 are connected by a pipeline, and the outer wall of the pipeline has a heat-insulating structure, such as a heat-insulating layer formed by a heat-insulating material.

[0035] It should be noted that after the reaction is completed, the product flows out from the bottom of the kettle and is transported to the flaker 20 through the pipeline. Since the reaction liquid is viscous, the hot fluid flowing through the outside of the pipeline cools down rapidly, the fluidity of the fluid decreases, and part of the product adheres to the pipe wall, resulting in loss. By setting a heat preservation structure on the outside of the pipeline, it is helpful to reduce the retention of the product in the pipeline.

[0036] The above-mentioned flaker can be purchased directly, and its specific structure can be set with reference to the existing technology, and no further elaboration or limitation is made here.

[0037] The production method of poly-cobalt provided by the present invention comprises the following steps: directly introducing the poly-cobalt material obtained by reacting di-tert-butyl peroxide and diisopropylbenzene in a reactor 10 into a flaker 20 including an immersion tank, a rotary drum and a scraper system; The poly-drying material introduced into the immersion tank is washed by the washing medium; the cooling medium is sprayed toward the drum by the spray system, so that the washed material adheres to the surface of the drum due to the cooling effect of the cooling medium during the rotation of the drum; the poly-drying product adhering to the surface of the drum is scraped off by the scraper system.

[0038] In some embodiments, before introducing the reaction raw materials, the equipment is first tested for tightness and purged with dry nitrogen, and the raw materials are introduced for reaction after the equipment operates normally.

[0039] In some embodiments, the reaction of di-tert-butyl peroxide and diisopropylbenzene in the reactor 10 includes: adding di-tert-butyl peroxide to diisopropylbenzene at a temperature of 130°C to 135°C (such as 130°C, 131°C, 132°C, 133°C, 134°C or 135°C) in the reactor 10 at a molar ratio of diisopropylbenzene to di-tert-butyl peroxide of 1:1 to 1:2 (such as 1:1, 1:1.5 or 1:2, etc.), until the content of di-tert-butyl peroxide in the reaction solution does not exceed 5wt%, and the reaction is stopped.

[0040] The introduction rate of the di-tert-butyl peroxide can be 400 mL / s to 400 mL / 2s.

[0041] If the di-tert-butyl peroxide dropwise acceleration is too fast, it will cause the loss of di-tert-butyl peroxide and affect the product yield.

[0042] The actual reaction temperature during the reaction process does not exceed 125°C.

[0043] As an example, the above reaction process can be referred to in the following manner: S1: Diisopropylbenzene is heated to about 80°C and enters the reactor 10, and the temperature is continuously raised to 130°C-135°C in the reactor 10.

[0044] S2: After the temperature in the kettle reaches the set temperature, maintain the temperature for 2 hours, and start dripping di-tert-butyl peroxide from the high-level tank 30, and the dripping rate of di-tert-butyl peroxide is maintained at 400mL / s~400mL / 2s. When distillate begins to be produced, the temperature of the reactor 10 is controlled to maintain the distillate rate at 40mL / s~20mL / s (taking a 2000L reactor 10 as an example), and the temperature in the kettle is controlled at about 120℃~125℃ (not exceeding 125℃). By controlling the dripping acceleration of the high-level tank 30, the loss of peroxide caused by the distillate being too fast is prevented.

[0045] S3: After all the di-tert-butyl peroxide in the high-level tank 30 is added dropwise, the temperature in the reactor 10 is maintained at 118° C. to 123° C., and sampling is performed through the manhole every 2 hours to monitor the reaction progress.

[0046] S4: After the reaction is kept warm for about 18h~22h, the liquid in the reactor 10 becomes viscous, and sampling is taken from the reactor 10 for testing. When the content of di-tert-butyl peroxide in the reaction liquid drops below 5%, the reaction is stopped, and the material discharged from the bottom of the reactor is introduced into the flaker 20.

[0047] After the reaction is completed, a washing agent (such as ethanol) is introduced into the immersion tank of the flaker 20, and a cooling medium (such as cooling water) is sprayed onto the drum through a spray system. The condensed matter will adhere to the surface of the drum. As the drum rotates, the scraper system scrapes the finished product off the drum and drops it into a material tray.

[0048] In some embodiments, the temperature of the cooling medium is 12°C to 18°C, such as 12°C, 13°C, 1°C, 15°C, 16°C, 17°C or 18°C, etc., or other values ​​within the range of 12°C to 18°C. In some preferred embodiments, the temperature of the cooling medium is 15°C.

[0049] It should be noted that in the post-processing unit, the cooling water at the inlet of the drum of the flaker 20 needs to be at a lower temperature. Therefore, it is necessary to increase the cooling water flow rate as the load increases while ensuring the minimum cooling water flow rate. If the minimum flow rate cannot be guaranteed, the cooling water at the outlet of the cooling nozzle cannot guarantee the spraying effect, which will cause uneven cooling water on the inner wall of the drum, and fail to meet the cooling requirements, and then fail to remove excess heat, and the product output efficiency decreases. The present invention can effectively meet the cooling requirements by setting the temperature of the cooling water introduced to 12°C~18°C, which is conducive to accelerating the output rate of the product.

[0050] In some embodiments, according to the reaction vessel 10 (the volume of the reaction vessel 10 may be 2m 3 ) to obtain 1.6m 3 The rotating speed of the drum can be set to 3 r / min to 5 r / min, such as 3 r / min, 3.5 r / min, 4 r / min, 4.5 r / min or 5 r / min, etc., or other values ​​within the range of 3 r / min to 5 r / min. In some preferred embodiments, the rotating speed of the drum is 4 r / min.

[0051] It should be noted that in the post-processing unit flaker 20, if the same speed is used for different outputs, the product may be too thick or too thin on the drum. If the distance between the scraper and the drum cannot be adjusted in time, the drum is easily scratched, seriously affecting production. The speed of the drum needs to be adapted to the output size. In this embodiment, the original multi-disc mechanical stepless speed change is adopted so that the machine can adapt to changes in output. If the output increases, the speed will be increased; if the output is small, the speed will be reduced. At the same time, the thickness of the flakes can be controlled. When the flakes are thicker, the speed will be reduced; when the flakes are thinner, the speed will be increased.

[0052] As above, after the reaction is completed, the hot fluid is discharged from the bottom of the reactor 10 and directly introduced into the flake machine 20. At the same time, the washing reagent is pumped into the immersion tank of the flake machine 20. The cooling medium is sprayed to the inner surface of the drum in a fan shape through the nozzle in the drum. When the liquid level in the immersion tank submerges the outer surface of the drum, the polylinked dry adheres to the outer surface of the drum when it is cold, and is taken away from the immersion tank as the drum rotates. It gradually cools and crystallizes on the outer surface of the drum, and rotates with the drum for one circle to the scraper. Because the surface of the drum is provided with a spiral groove, it is scraped off by the blade when passing through the knife holder device, falls into the inlet and outlet groove, and flows to the packaging production line. This process does not need to stir and precipitate the reaction product, which eliminates the operation steps of stirring and precipitating in the stirring kettle in the prior art, and then passing through the plate and frame filter press or centrifuge separation, saving construction costs and reducing operation steps. In addition, since the flake machine 20 uses ethanol and cooling water, it also solves the problem that ice ethanol is difficult to store in the prior art. The finished product is directly discharged and falls into the material tray, which greatly improves production efficiency.

[0053] The above method realizes the continuous preparation of poly-anthate, which is not only simple to operate and has high production efficiency, but also improves the yield and purity of the obtained poly-anthate product, effectively solving the problem of low yield of current batch reaction process, and has high industrial application value.

[0054] The features and performance of the present invention are further described in detail below in conjunction with the embodiments.

[0055] Example 1 This embodiment provides a production system of polylinked dry products, such as Figure 1 As shown, it includes a polymerization unit and a post-processing unit.

[0056] The polymerization unit includes a reactor 10. The top of the reactor 10 has a first inlet 11 for introducing diisopropylbenzene and a second inlet 12 for introducing di-tert-butyl peroxide. The first inlet 11 is connected to the di-tert-butyl peroxide storage tank, and the second inlet 12 is connected to the di-tert-butyl peroxide storage tank. An overhead tank 30 is also connected between the di-tert-butyl peroxide storage tank and the second inlet 12 of the reactor 10. An anchor-type stirring paddle is provided in the reactor 10, and the reactor 10 also has a jacket. The top of the reactor 10 is connected to a shell-and-tube heat exchanger 40, and the shell-and-tube heat exchanger is connected to a recovery tank 50.

[0057] The post-processing unit includes a flaker 20 and a spray system. The flaker 20 includes an immersion tank, a rotary drum, a scraper system and a material tray. The bottom of the reactor 10 is connected to the immersion tank of the flaker 20 through a pipeline, and the outer wall of the pipeline is provided with an insulation layer formed by an insulation material. The immersion tank of the flaker 20 is also connected to an ethanol storage tank. The nozzle of the spray system faces the rotary drum, and a spiral groove is provided on the surface of the rotary drum. The scraper system is used to scrape off the solid material attached to the surface of the rotary drum and drop it into the material tray.

[0058] Example 2 This embodiment provides a method for producing polylinkerol, comprising: S1: Diisopropylbenzene is heated to about 80°C and introduced into the reactor 10, and the temperature is continuously raised to 135°C in the reactor 10.

[0059] S2: After the temperature in the kettle reaches the set temperature, maintain the temperature for 2 hours, and start dripping di-tert-butyl peroxide from the high-level tank 30 at a molar ratio of diisopropylbenzene to di-tert-butyl peroxide of 1:2, and maintain the dripping rate of di-tert-butyl peroxide at 400 mL / s. When distillate begins to be produced, the temperature of the reactor 10 is controlled to maintain the distillate rate at 40 mL / s (taking a 2000L reactor 10 as an example), and the temperature in the reactor is controlled at about 120°C~125°C.

[0060] S3: After all the di-tert-butyl peroxide in the high-level tank 30 is added dropwise, the temperature in the reactor 10 is maintained at 118° C. to 123° C., and sampling is performed through the manhole every 2 hours to monitor the reaction progress.

[0061] S4: After the reaction is kept warm for about 20 hours, samples are taken from the reactor 10 for testing. When the content of di-tert-butyl peroxide in the reaction solution drops below 5%, the reaction is stopped and the material discharged from the bottom of the reactor is introduced into the flaker 20.

[0062] S5: Ethanol is introduced into the immersion tank of the flaker 20, and the spray device sprays cooling water with a temperature of 15°C onto the drum. The poly-dextrose is attached to the surface of the drum. As the drum rotates (4r / min), the scraper system scrapes the finished product off the drum and drops it into the material tray.

[0063] Example 3 This embodiment provides a method for producing polylinkerol, comprising: S1: Diisopropylbenzene is heated to about 80°C and enters the reactor 10, and the temperature is continuously raised to 130°C in the reactor 10.

[0064] S2: After the temperature in the kettle reaches the set temperature, maintain the temperature for 2 hours, and start dripping di-tert-butyl peroxide from the high-level tank 30 at a molar ratio of diisopropylbenzene to di-tert-butyl peroxide of 1:1.5. The dripping rate of di-tert-butyl peroxide is maintained at 400mL / 2s. When distillate begins to be produced, the temperature of the reactor 10 is controlled to maintain the distillate rate at 20mL / s (taking a 2000L reactor 10 as an example). At this time, the temperature in the kettle is controlled at about 120℃~125℃ (not exceeding 125℃). By controlling the dripping acceleration of the high-level tank 30, the loss of peroxide caused by the distillate being too fast is prevented.

[0065] S3: After all the di-tert-butyl peroxide in the high-level tank 30 is added dropwise, the temperature in the reactor 10 is maintained at 118° C. to 123° C., and sampling is performed through the manhole every 2 hours to monitor the reaction progress.

[0066] S4: After the reaction is kept warm for about 18 hours, the liquid in the reactor 10 becomes viscous, and sampling is performed in the reactor 10 for testing. When the content of di-tert-butyl peroxide in the reaction liquid drops below 5%, the reaction is stopped, and the material discharged from the bottom of the reactor is introduced into the flaker 20.

[0067] S5: Ethanol is introduced into the immersion tank of the flaker 20, and the spray device sprays cooling water with a temperature of 12°C onto the drum. The poly-dextrose is attached to the surface of the drum. As the drum rotates (3r / min), the scraper system scrapes the finished product off the drum and drops it into the material tray.

[0068] Example 4 This embodiment provides a method for producing polylinkerol, comprising: S1: Diisopropylbenzene is heated to about 80°C and enters the reactor 10, and the temperature is continuously raised to 132°C in the reactor 10.

[0069] S2: After the temperature in the kettle reaches the set temperature, maintain the temperature for 2 hours, and start dripping di-tert-butyl peroxide from the high-level tank 30 at a molar ratio of diisopropylbenzene to di-tert-butyl peroxide of 1:1. The dripping rate of di-tert-butyl peroxide is maintained at 400mL / 1.5s. When distillate begins to be produced, the temperature of the reactor 10 is controlled to maintain the distillate rate at 40mL / 1.5s (taking a 2000L reactor 10 as an example). At this time, the temperature in the kettle is controlled at about 120℃~125℃ (not exceeding 125℃). By controlling the dripping acceleration of the high-level tank 30, the loss of peroxide caused by the distillate being too fast is prevented.

[0070] S3: After all the di-tert-butyl peroxide in the high-level tank 30 is added dropwise, the temperature in the reactor 10 is maintained at 118° C. to 123° C., and sampling is performed through the manhole every 2 hours to monitor the reaction progress.

[0071] S4: After the reaction is kept warm for about 22 hours, the liquid in the reactor 10 becomes viscous, and sampling is performed in the reactor 10 for testing. When the content of di-tert-butyl peroxide in the reaction liquid drops below 5%, the reaction is stopped, and the material discharged from the bottom of the reactor is introduced into the flaker 20.

[0072] S5: Ethanol is introduced into the immersion tank of the flaker 20, and the spray device sprays cooling water with a temperature of 18°C ​​onto the drum. The poly-dextrose is attached to the surface of the drum. As the drum rotates (5r / min), the scraper system scrapes the finished product off the drum and drops it into the material tray.

[0073] Comparative Example 1 The difference between this comparative example and Example 2 is that the reactor 10 is not provided with a jacket for passing steam, and the temperature is not controlled by controlling the steam flow rate during the reaction process.

[0074] Comparative Example 2 The difference between this comparative example and Example 2 is that the dropping rate of di-tert-butyl peroxide is maintained at 400 mL / 0.5 s.

[0075] Comparative Example 3 The difference between this comparative example and Example 2 is that no insulation layer is provided on the outside of the pipe connecting the bottom of the reactor 10 and the immersion tank of the flaker 20 .

[0076] Comparative Example 4 The difference between this comparative example and Example 2 is that the temperature of the cooling water is 10°C.

[0077] Comparative Example 5 The difference between this comparative example and Example 2 is that the temperature of the cooling water is 20°C.

[0078] Comparative Example 6 The difference between this comparative example and Example 2 is that the rotating speed of the drum is 2 r / min.

[0079] Comparative Example 7 The difference between this comparative example and Example 2 is that the rotating speed of the drum is 6 r / min.

[0080] Comparative Example 8 The difference between this comparative example and Example 2 is that: the conventional method is adopted to introduce the bottom discharge of the reactor 10 into the stirring reactor with insulation, and after stirring and precipitation, the solid-liquid separation is carried out by a plate and frame filter press.

[0081] Test example The product yield, product purity and production efficiency of the above Examples 2 to 4 and Comparative Examples 1 to 8 were compared, and the results are shown in Table 1.

[0082] Table 1 Comparison results

[0083] It can be seen from Table 1 that the method provided by the present invention can improve production efficiency while obtaining poly-linked oligomer with high yield and purity.

[0084] In summary, the production method of poly-anthate provided by the present invention realizes the continuous preparation of poly-anthate, which is not only simple to operate and has high production efficiency, but also improves the yield and purity of the obtained poly-anthate product, effectively solving the problem of low yield of current batch reaction processes, and has high industrial application value.

[0085] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for producing polyunsaturated fat, characterized in that: The method comprises the following steps: directly introducing the polycondensed material obtained by reacting di-tert-butyl peroxide and diisopropylbenzene in a reactor into a flaker including an immersion tank, a rotary drum and a scraper system; The poly-deoxycarbonate material introduced into the immersion tank is washed by a washing medium; a cooling medium is sprayed toward the drum by a spray system, so that the washed material adheres to the surface of the drum due to the cooling effect of the cooling medium during the rotation of the drum; the poly-deoxycarbonate product adhering to the surface of the drum is scraped off by the scraper system; The reactor is provided with an anchor-type stirring paddle; the reactor has a jacket; The reactor and the flaker are connected by a pipeline, and the outer wall of the pipeline has a heat-insulating structure; The temperature of the cooling medium is 12°C to 18°C; According to the reaction kettle, 1.6m 3 For the polymerized dry materials, the speed of the drum is 3r / min~5r / min.

2. The production method according to claim 1, characterized in that The reaction of di-tert-butyl peroxide and diisopropylbenzene in a reactor comprises: adding di-tert-butyl peroxide to diisopropylbenzene at a temperature of 130° C. to 135° C. in a reactor at a molar ratio of the diisopropylbenzene to the di-tert-butyl peroxide of 1:1 to 1:2, until the content of di-tert-butyl peroxide in the reaction solution does not exceed 5wt%, and then stopping the reaction.

3. The production method according to claim 2, characterized in that: The introduction rate of the di-tert-butyl peroxide is 400 mL / s to 400 mL / 2s.

4. The production method according to claim 3, characterized in that: The actual reaction temperature during the reaction process does not exceed 125°C.

5. The production method according to any one of claims 1 to 4, characterized in that: The top of the reactor is connected with a shell and tube heat exchanger to perform heat exchange and recovery on the gas evaporated from the top of the reactor.

Citation Information

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