Method for granulating 5-iodouridine by using fluororubber F2311

Abstract

The invention discloses a method for granulating 5-iodouridine by using fluororubber F2311, and belongs to the technical field of fluororubber and energetic material granulation, and the method comprises the following steps: preparing a 5-iodouridine suspension, and preparing a fluororubber F2311 solution by using the fluororubber F2311; and dropwise adding a fluororubber F2311 solution into the 5-iodouridine suspension, raising the temperature after dropwise adding, keeping a certain rotation speed, and evaporating the solvent to dryness to prepare the fluororubber F2311 coated and granulated 5-iodouridine. According to the invention, 5-iodouridine is granulated by using a water suspension method, and after fluororubber F2311 is coated and granulated, the particle size of the 5-iodouridine is remarkably reduced, and the dispersity of the 5-iodouridine is relatively uniform, so that the 5-iodouridine is favorably dispersed in other substances. The fluororubber F2311 has good heat resistance and corrosion resistance, and after the fluororubber F2311 is combined with the 5-iodouridine, the stability of the compound can be greatly enhanced, so that the compound is more difficult to decompose or denature.

Description

Technical Field

[0001] The invention belongs to the technical field of granulation of fluororubber and energetic materials, and more specifically, the invention relates to a method for granulating 5-iodouridine by using fluororubber F2311. Background Art

[0002] It is very dangerous to directly study energetic materials such as HMX in experiments such as pressing. If we first use substitutes with similar properties to conduct experimental exploration, and obtain experimental conditions close to the correct conditions, and then use energetic materials such as HMX to conduct experiments, the danger can be greatly reduced and the success rate of the experiment can be improved. Therefore, it is very meaningful to conduct experiments with substitutes. A granulation experiment was conducted on a substitute for HMX, and the optimal experimental conditions for the granulation of the substitute were obtained. After the discussion, it was also helpful for the granulation of HMX. And studying how to prepare modeling powder can first improve the thermal stability of energetic materials. Energetic materials can cause spontaneous combustion or explosion under high temperature and high pressure conditions. Studies have found that adding an appropriate amount of modeling powder can improve the thermal stability of energetic materials and increase their thermal instability temperature, thereby improving their safety and application effect. Secondly, it can strengthen the mechanical properties of the material. Modeling powder can make energetic materials have better mechanical stability during combustion or explosion, and tensile strength, thermal conductivity and electrical properties can also be improved, which helps to improve the molding ability and application performance of energetic materials. It can also improve the combustion performance of energetic materials. Modeling powder can change the combustion process of energetic materials and the generation of combustion products, making them have better performance, such as increasing the burning rate and reducing the combustion temperature, which helps to improve the energy density and combustion efficiency of energetic materials. Finally, explore new methods for preparing energetic materials. Studying the synthesis process and special properties of modeling powder can provide new ideas for the preparation of energetic materials and promote technological progress and development in the field of energetic materials. Therefore, studying the application of modeling powder in the field of energetic materials is of great significance, which can improve the performance and application effect of energetic materials and promote the scientific research development and industrial application of energetic materials.

[0003] Using safe materials to simulate HMX has important research value and practical significance. However, the simulation materials used in the past, such as melamine, sucrose, millet, etc., have different disadvantages, such as low density, large difference in mechanical properties, poor compression performance, etc., and adding heavy metal salts to increase the density will cause new problems. In order to solve the above problems, the present invention uses 5-iodouridine as a substitute for HMX. The chemical formula of 5-iodouridine is C9H 11IN2O6 is stable at room temperature and pressure, and its crystal properties are very similar to those of HMX. The basic properties of 5-iodouridine are that it is insoluble in ethanol, ethyl acetate, n-hexane, cyclohexane, and acetone. Zhan Chunhong et al. studied the effects of HMX particle characteristics on the coating and molding of PBX explosives. Through their research, it can be inferred that the more dispersed and finer the 5-iodouridine crystals are, the better the coating and granulation effect will be. During granulation, the raw material properties and manufacturing process parameters usually affect the granulation effect. Fluororubber F2311 can not only be used as a desensitizer and explosive carrier in the process of granulating energetic materials, but its main function is bonding, which directly affects the granulation of molding powder. At present, there are three basic methods for granulating energetic materials, namely water suspension method, kneading method, and emulsion coating method. Summary of the invention

[0004] An object of the present invention is to solve at least the above problems and / or disadvantages and to provide at least the advantages which will be described hereinafter.

[0005] In order to achieve these purposes and other advantages according to the present invention, a method for granulating 5-iodouridine using fluororubber F2311 is provided, characterized in that it comprises the following steps:

[0006] Step 1: prepare 5-iodouridine suspension, and use fluororubber F2311 to prepare fluororubber F2311 solution;

[0007] Step 2: Add the fluororubber F2311 solution to the 5-iodouridine suspension at a certain rotation speed and a certain dropping speed, maintain the solution for a certain time after the addition is completed, then increase the temperature, maintain a certain rotation speed, evaporate the solvent, and prepare 5-iodouridine coated with fluororubber F2311 granules.

[0008] Preferably, in the step 1, the method for preparing the 5-iodouridine suspension comprises: placing 5-iodouridine in ethanol, ultrasonicating for 2 to 10 minutes, and then stirring at an initial temperature of 40°C to 55°C and a speed of 200 to 500 rpm for 5 to 15 minutes to obtain a uniform 5-iodouridine suspension; wherein the mass ratio of 5-iodouridine to ethanol is 1:8 to 20.

[0009] Preferably, in the step 1, the fluororubber F2311 is a copolymer of chlorotrifluoroethylene and chloroethyleneidene fluoride.

[0010] Preferably, in step one, the method of preparing a fluororubber F2311 solution using fluororubber F2311 comprises: dissolving fluororubber F2311 in ethyl acetate, wherein the mass ratio of fluororubber F2311 to ethyl acetate is 2-5:95-98, and the mass ratio of 5-iodouridine to fluororubber F2311 is 94-97:3-6.

[0011] Preferably, in the step 2, the rotation speed of dripping the fluororubber F2311 solution is 200-600 rpm, the dripping temperature is 40-60°C, the evaporation rotation speed is 300-500 rpm, and the evaporation temperature is 50-65°C.

[0012] Preferably, the dropping speed of the fluororubber F2311 solution is 0.3-0.9 mL / s.

[0013] Preferably, the step 1 and the step 2 are replaced by: placing 5-iodouridine in a certain proportion of ethanol, ultrasonicating for 2 to 10 minutes, and then granulating at 300 to 600 rpm at a certain temperature for 5 to 15 minutes; raising the temperature to a certain temperature, adding the fluororubber F2311 solution at a certain speed and a certain dropping speed, keeping it for 1 to 3 minutes after the addition is completed, then raising the temperature and changing the speed to evaporate, stopping the evaporation when only half of the liquid has evaporated, cooling to room temperature, and filtering to obtain 5-iodouridine coated with fluororubber F2311 granules.

[0014] Preferably, the rotation speed of dropping the fluororubber F2311 solution is 150-500 rpm, and the dropping temperature is 40-55° C.; the evaporation rotation speed is 200-550 rpm, and the evaporation temperature is 50-65° C.

[0015] Preferably, the solvent of the fluororubber F2311 solution is acetone, and the mass ratio of fluororubber F2311 to acetone is 2-5:95-98.

[0016] Preferably, the mass ratio of 5-iodouridine to ethanol is 1:10-20: the mass ratio of 5-iodouridine to fluororubber F2311 is 94-97:3-6.

[0017] In order to improve the flowability of 5-iodouridine and reduce the particle size and particle size distribution range of 5-iodouridine, the fluororubber F2311 used in step 2 is replaced by modified fluororubber F2311; wherein the preparation method of modified fluororubber F2311 comprises:

[0018] S1. Add an emulsifier to deionized water, and stir at a speed of 1200 to 2400 rpm for 1 to 3 hours to obtain an emulsified system; wherein the emulsifier is one of perfluoropolyether (meth)acrylate, sodium trifluoromethanesulfonate, and perfluorobutylsulfonic acid triphenylsulfonium salt;

[0019] S2, add the emulsified system into the reactor, and evacuate the reactor to 1.2×10 -2Pa, heating the emulsified system to 60-70°C, then adding vinylidene fluoride and chlorotrifluoroethylene into the emulsified system in a ratio of 1:1, adding an oxidant, a reducing agent and maleic anhydride in batches while stirring and mixing, pressurizing to 2.2-3.6MPa, and heating to 80-90°C to carry out polymerization reaction, after reacting for 5-10 hours, releasing the pressure, cooling to 0-4°C to obtain fluororubber F2311;

[0020] The oxidant is one of potassium persulfate, ammonium persulfate and potassium permanganate, the reducing agent is one of sodium bisulfite, sulfur trioxide, sodium bromide and potassium bromide, and the mass ratio of deionized water, emulsifier, oxidant, reducing agent, maleic anhydride and vinylidene fluoride is 500-1000: 0.002-10: 0.005-15: 0.001-5: 10-30: 64-192;

[0021] S3, using Ar plasma to modify the prepared fluororubber F2311, the specific method includes:

[0022] The fluororubber F2311 was cut into thin sheets with a thickness of 0.1 to 0.3 mm. The thin sheets were washed with deionized water and placed in a vacuum chamber with a degree of vacuum of 2.5 × 10 -6 In a vacuum chamber below Pa, Ar gas is introduced into the vacuum chamber, the flow rate of Ar gas is 12-18 sccm, the radio frequency frequency is 10-80 MHz, the voltage is 300-800 V, and Ar plasma directly acts on the thin film to modify the thin film. The modification treatment time is 1-3 hours. After taking out, the thin film is crushed to obtain modified fluororubber F2311.

[0023] The present invention at least includes the following beneficial effects: the present invention uses a water suspension method to granulate 5-iodouridine, and determines the optimal conditions for granulating 5-iodouridine. The experimental temperature is 65°C, and the mass ratio of 5-iodouridine and solvent (ethanol) is 1:13; the mass ratio of fluororubber F2311 to ethyl acetate or acetone is 5:95; the mass ratio of 5-iodouridine to fluororubber F2311 is 95:5, the feeding rate is 0.8mL / s, and the stirring rate is 200r / min. After the fluororubber F2311 is coated and granulated, the particle size of 5-iodouridine is significantly reduced and the dispersion of 5-iodouridine is relatively uniform, which is conducive to dispersion in other substances. This can also strengthen the protection of 5-iodouridine and prevent it from being affected by adverse environments during storage or use and failing. Fluororubber F2311 fluororubber itself has good heat resistance and corrosion resistance. After combining with 5-iodouridine, the stability of the compound can be greatly enhanced, making it more difficult to be decomposed or denatured.

[0024] The invention discloses a preparation method of modified fluororubber F2311, and uses the modified fluororubber F2311 to coat and granulate 5-iodouridine. The results show that after maleic anhydride is added during the preparation process and Ar plasma is used for modification, the modified fluororubber F2311 has a better coating and granulation effect on 5-iodouridine, significantly improves the flowability of 5-iodouridine, and reduces the particle size and particle size distribution range of 5-iodouridine particles.

[0025] Other advantages, objectives and features of the present invention will be embodied in part through the following description, and in part will be understood by those skilled in the art through study and practice of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 This is the SEM image of 5-iodouridine in the 2 μm particle size range without fluororubber F2311 coating and granulation;

[0027] Figure 2 This is the SEM image of 5-iodouridine in the particle size range of 10 μm without fluororubber F2311 coating and granulation;

[0028] Figure 3 This is the SEM image of 5-iodouridine in the particle size range of 20 μm without fluororubber F2311 coating and granulation;

[0029] Figure 4 This is a SEM image of 5-iodouridine in the particle size range of 10 μm after being coated and granulated with fluororubber F2311 in Example 37;

[0030] Figure 5 This is a SEM image of 5-iodouridine in the particle size range of 20 μm after being coated and granulated with fluororubber F2311 in Example 37;

[0031] Figure 6 This is a SEM image of 5-iodouridine in the particle size range of 100 μm after being coated and granulated with fluororubber F2311 in Example 37;

[0032] Figure 7 The infrared spectra of 5-iodouridine coated and granulated with fluororubber F2311 and raw material 5-iodouridine in Example 37;

[0033] Figure 8 This is the XRD spectrum of 5-iodouridine coated with fluororubber F2311 and raw material 5-iodouridine in Example 37. DETAILED DESCRIPTION

[0034] The present invention is further described in detail below in conjunction with the accompanying drawings so that those skilled in the art can implement the invention with reference to the description.

[0035] It should be understood that the terms such as “having”, “including” and “comprising” used herein do not exclude the existence or addition of one or more other elements or combinations thereof.

[0036] Example 1

[0037] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311, comprising the following steps:

[0038] Step 1, 0.95 g of 5-iodouridine is placed in 14.25 g of ethanol, ultrasonicated for 5 min, and then stirred at an initial temperature of 55° C. and a speed of 400 rpm for 10 min to obtain a uniform 5-iodouridine suspension; fluororubber F2311 is selected as fluororubber F2311, wherein fluororubber F2311 is a copolymer of trifluoroethylene and vinylidene fluoride, and 0.05 g of fluororubber F2311 is dissolved in 0.95 g of ethyl acetate to obtain a fluororubber F2311 solution;

[0039] Step 2: At a rotation speed of 400 rpm, add the fluororubber F2311 solution to the 5-iodouridine suspension at a dropping speed of 0.8 mL / s, the initial dropping temperature is 55°C, and the dropping is maintained for 1 min after the addition is completed. Then the temperature is increased to 65°C, and the evaporation speed is maintained at 300 rpm to evaporate the solvent to prepare fluororubber F2311-coated granulated 5-iodouridine.

[0040] In this embodiment, the 5-iodouridine granules were coated with fluororubber F2311 and the effect was good.

[0041] Example 2

[0042] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that the dripping speed of the fluororubber F2311 solution in step 2 of this embodiment is 0.3 mL / s, and the method parameters of the remaining steps are the same as those in Example 1.

[0043] The 5-iodouridine in this example was not granulated, and the fluororubber F2311 was in agglomerates.

[0044] Example 3

[0045] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that the dripping speed of the fluororubber F2311 solution in step 2 of this embodiment is 0.4 mL / s, and the method parameters of the remaining steps are the same as those in Example 1.

[0046] The 5-iodouridine in this example was not granulated, and the fluororubber F2311 was in agglomerates.

[0047] Example 4

[0048] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that the dripping speed of the fluororubber F2311 solution in step 2 of this embodiment is 0.5 mL / s, and the method parameters of the remaining steps are the same as those in Example 1.

[0049] The 5-iodouridine in this example was not granulated, and the fluororubber F2311 was in agglomerates.

[0050] Example 5

[0051] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that the dripping speed of the fluororubber F2311 solution in step 2 of this embodiment is 0.6 mL / s, and the method parameters of the remaining steps are the same as those in Example 1.

[0052] The 5-iodouridine in this example was granulated but the effect was poor, and a lot of 5-iodouridine was not granulated.

[0053] Example 6

[0054] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that the dripping speed of the fluororubber F2311 solution in step 2 of this embodiment is 0.7 mL / s, and the method parameters of the remaining steps are the same as those in Example 1.

[0055] The 5-iodouridine in this example was granulated, but the particles were relatively large.

[0056] Example 7

[0057] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that the dripping speed of the fluororubber F2311 solution in step 2 of this embodiment is 0.9 mL / s, and the method parameters of the remaining steps are the same as those in Example 1.

[0058] Through the comparison of Examples 1 to 7, it was found that the coating effect of the ethyl acetate solution of fluororubber F2311 was significantly improved when the dropping speed was 0.8 mL / s and 0.9 mL / s compared with other speeds. The specific situation should be that the dropping speed was too low, the fluororubber F2311 was broken up, so it could not be coated with the drug, and the dropping speed was too fast, the fluororubber F2311 was not broken up, and agglomerated and precipitated.

[0059] The 5-iodouridine in this example was granulated but the effect was poor and the particles were relatively large.

[0060] Example 8

[0061] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that the initial dropping temperature of the fluororubber F2311 solution in step 2 is 40°C, the evaporation temperature is 50°C, and the method parameters of the remaining steps are the same as those in Example 1.

[0062] The granulation effect of 5-iodouridine in this example is poor, and much 5-iodouridine is not coated with fluororubber F2311.

[0063] Example 9

[0064] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that the initial dropping temperature of the fluororubber F2311 solution in step 2 is 45°C, the evaporation temperature is 55°C, and the method parameters of the remaining steps are the same as those in Example 1.

[0065] The granulation effect of 5-iodouridine in this example is poor, and much 5-iodouridine is not coated with fluororubber F2311.

[0066] Example 10

[0067] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that the initial dropping temperature of the fluororubber F2311 solution in step 2 is 50°C, the evaporation temperature is 60°C, and the method parameters of the remaining steps are the same as those in Example 1.

[0068] The granulation effect of 5-iodouridine in this example is average, and there is still a lot of 5-iodouridine not coated with fluororubber F2311.

[0069] By comparing Example 1, Example 8, Example 9 and Example 10, when the addition temperature is 55°C and the evaporation temperature is 65°C, the coating granulation effect is the best. If the evaporation temperature is not high enough, the evaporation rate is not enough and it is difficult for the fluororubber F2311 to precipitate.

[0070] Embodiment 11

[0071] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that in step 1, the mass of fluororubber F2311 is 0.05 g, the mass of ethyl acetate is 2.45 g, and the method parameters of the remaining steps are the same as those in Example 1.

[0072] The 5-iodouridine in this example was substantially not granulated.

[0073] Example 12

[0074] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that in step 1, the mass of fluororubber F2311 is 0.05 g, the mass of ethyl acetate is 1.62 g, and the method parameters of the remaining steps are the same as those in Example 1.

[0075] In this example, 5-iodouridine was partially granulated, but many of them were not granulated.

[0076] Example 13

[0077] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that in step 1, the mass of fluororubber F2311 is 0.05 g, the mass of ethyl acetate is 1.2 g, and the method parameters of the remaining steps are the same as those in Example 1.

[0078] The 5-iodouridine in this example is granulated and has moderate granularity, and has a better granular feel than that in Example 12.

[0079] By comparing Example 1, Example 11, Example 12 and Example 13, when the mass ratio of fluororubber F2311 to ethyl acetate is 5:95, the coating effect is better than other mass ratios. The higher the mass ratio of fluororubber F2311 to ethyl acetate, the greater the evaporation rate, making it easier for fluororubber F2311 to precipitate, and the more fluororubber F2311, the better the coating effect in theory.

[0080] Embodiment 14

[0081] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that the amount of 5-iodouridine used in step 1 is 0.95 g, the amount of ethanol used is 9.5 g, and the method parameters of the remaining steps are the same as those in Example 1.

[0082] The granulation effect of 5-iodouridine in this example is not good, and basically no granulation is formed.

[0083] Embodiment 15

[0084] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that the amount of 5-iodouridine used in step 1 is 0.95 g, the amount of ethanol used is 12.35 g, and the method parameters of the remaining steps are the same as those in Example 1.

[0085] The 5-iodouridine in this example granulated well and the particles were moderate.

[0086] Example 16

[0087] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that the amount of 5-iodouridine used in step 1 is 0.95 g, the amount of ethanol used is 16.15 g, and the method parameters of the remaining steps are the same as those in Example 1.

[0088] The 5-iodouridine in this example was granulated but the particles were relatively large.

[0089] Embodiment 17

[0090] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that the amount of 5-iodouridine used in step 1 is 0.95 g, the amount of ethanol used is 18.05 g, and the method parameters of the remaining steps are the same as those in Example 1.

[0091] The 5-iodouridine in this example did not granulate.

[0092] Embodiment 18

[0093] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that the amount of 5-iodouridine used in step 1 is 0.95 g, the amount of ethanol used is 19 g, and the method parameters of the remaining steps are the same as those in Example 1.

[0094] The 5-iodouridine in this example did not granulate.

[0095] Embodiment 19

[0096] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 1, the difference is that the amount of 5-iodouridine used in step 1 is 0.95 g, the amount of ethanol used is 7.6 g, and the method parameters of the remaining steps are the same as those in Example 1.

[0097] The 5-iodouridine in this example did not granulate.

[0098] Through the comparison between Example 1 and Example 14 to Example 19, the granulation effect when the mass ratio of 5-iodouridine to ethanol is controlled at about 1:15 is better than that of the other mass ratios.

[0099] Embodiment 20

[0100] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311, comprising the following steps:

[0101] Step 1, 0.97 g of 5-iodouridine is placed in 9.7 g of ethanol, ultrasonicated for 5 min, and then stirred at an initial temperature of 55° C. and a speed of 400 rpm for 10 min to obtain a uniform 5-iodouridine suspension; fluororubber F2311 is selected as fluororubber F2311, wherein fluororubber F2311 is a copolymer of trifluoroethylene and vinylidene fluoride, and 0.03 g of fluororubber F2311 is dissolved in 0.97 g of ethyl acetate to obtain a fluororubber F2311 solution;

[0102] Step 2: At a rotation speed of 250 rpm, add the fluororubber F2311 solution to the 5-iodouridine suspension at a dropping speed of 0.8 mL / s. The initial dropping temperature is 55°C. After the addition is completed, keep it for 1 min, then increase the temperature to 60°C, maintain the evaporation speed of 300 rpm, evaporate the solvent, and prepare fluororubber F2311-coated granulated 5-iodouridine.

[0103] The 5-iodouridine in this example was not granulated.

[0104] Embodiment 21

[0105] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 20, the difference is that the dripping speed of fluororubber F2311 is 300 rpm, the evaporation speed is 350 rpm, and the method parameters of the remaining steps are the same as those of Example 21.

[0106] The 5-iodouridine in this example was not granulated.

[0107] Embodiment 22

[0108] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 20, the difference is that the dripping speed of fluororubber F2311 is 400 rpm, the evaporation speed is 450 rpm, and the method parameters of the remaining steps are the same as those of Example 21.

[0109] The 5-iodouridine in this example did not granulate.

[0110] Embodiment 23

[0111] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 20, the difference is that the dripping speed of fluororubber F2311 is 250 rpm, the evaporation speed is 400 rpm, and the method parameters of the remaining steps are the same as those of Example 21.

[0112] The 5-iodouridine in this example did not granulate.

[0113] Embodiment 23

[0114] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 20, the difference is that the dripping speed of fluororubber F2311 is 450 rpm, the evaporation speed is 500 rpm, and the method parameters of the remaining steps are the same as those of Example 21.

[0115] The 5-iodouridine in this example forms small particles.

[0116] Embodiment 24

[0117] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311, comprising the following steps:

[0118] Step 1, 0.96 g of 5-iodouridine is placed in 9.6 g of ethanol, ultrasonicated for 5 min, and then stirred at an initial temperature of 55° C. and a speed of 400 rpm for 10 min to obtain a uniform 5-iodouridine suspension; fluororubber F2311 is selected as fluororubber F2311, wherein fluororubber F2311 is a copolymer of trifluoroethylene and vinylidene fluoride, and 0.04 g of fluororubber F2311 is dissolved in 0.96 g of ethyl acetate to obtain a fluororubber F2311 solution;

[0119] Step 2: At a rotation speed of 450 rpm, add the fluororubber F2311 solution to the 5-iodouridine suspension at a dropping speed of 0.8 mL / s. The initial dropping temperature is 55°C. After the addition is completed, keep it for 1 min, then increase the temperature to 60°C, maintain the evaporation speed of 500 rpm, evaporate the solvent, and prepare 5-iodouridine coated with fluororubber F2311 granules.

[0120] The 5-iodouridine in this example was granulated but the granularity was not obvious and the fluororubber F2311 was in lumps.

[0121] Embodiment 25

[0122] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 24, the difference is that the rotation speed of the fluororubber F2311 solution during dripping in step 2 is 500 rpm, the evaporation speed is 300 rpm, and the method parameters of the remaining steps are the same as those of Example 26.

[0123] The 5-iodouridine in this example was granulated but the granularity was not obvious and the fluororubber F2311 was in lumps.

[0124] Embodiment 26

[0125] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 24, the difference is that the rotation speed of the fluororubber F2311 solution during dropwise addition in step 2 is 550 rpm, the evaporation speed is 300 rpm, and the method parameters of the remaining steps are the same as those of Example 26.

[0126] The 5-iodouridine in this example was granulated but the granularity was not obvious and the fluororubber F2311 was in lumps.

[0127] Embodiment 27

[0128] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. Compared with Example 25, the difference is that the rotation speed of the fluororubber F2311 solution during dripping in step 2 is 400 rpm, the evaporation speed is 300 rpm, and the method parameters of the remaining steps are the same as those of Example 26.

[0129] The 5-iodouridine in this example was granulated with obvious granularity, but the fluororubber F2311 was in blocks.

[0130] By the comparison of embodiment 20-embodiment 23, embodiment 25-embodiment 27, it can be seen that when the mass ratio of 5-iodouridine: fluororubber F2311 is 96:4, the addition speed is 450rpm, and the granulation effect of the evaporation speed is 500rpm is more excellent than the product coating effect under the condition of mass ratio 97:3 and the same speed, and the particle size of its product is more refined. When the speed is changed to add a speed of 400rpm, the coating effect is improved after the evaporation speed of 300rpm, and its product particles are more granular. In the case of evaporating the solvent, the speed can basically determine that adding a speed of 300rpm and an evaporation speed of 400rpm are more excellent than adding a speed of 450rpm and an evaporation speed of 550rpm. Without changing the rotation speed, the mass ratio of iodouridine:fluororubber F2311 of 95:5 is better than 96:4, and the maximum mass ratio is 95:5. Therefore, it is determined that 5-iodouridine:fluororubber F2311=95:5 is the best granulation mass ratio, and the addition speed of 300rpm and the evaporation speed of 400rpm are the best speeds.

[0131] When the evaporation solvent method was finally used, the mass ratio of 5-iodouridine to ethanol was 1:15, the mass ratio of 5-iodouridine to fluororubber F2311 was 95:5, the addition speed and evaporation speed were 400 rpm and 300 rpm respectively, the mass ratio of fluororubber F2311 to ethyl acetate was 5:95, the addition temperature was 55°C, the evaporation temperature was 65°C, and the dripping acceleration of the fluororubber F2311 solution was 0.8 mL / s, and the coating effect was the best.

[0132] Embodiment 28

[0133] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311, comprising the following steps:

[0134] Step 1, 0.95 g of 5-iodouridine is placed in 14.25 g of ethanol, ultrasonicated for 5 min, and then stirred at an initial temperature of 55° C. and a speed of 500 rpm for 10 min to obtain a uniform 5-iodouridine suspension; fluororubber F2311 is selected as fluororubber F2311, wherein fluororubber F2311 is a copolymer of trifluoroethylene and vinylidene fluoride, and 0.05 g of fluororubber F2311 is dissolved in 0.95 g of acetone to obtain a fluororubber F2311 solution;

[0135] Step 2: Raise the temperature to 55°C, add the fluororubber F2311 solution to the 5-iodouridine suspension at a dropping speed of 0.8 mL / s at a rotation speed of 150 rpm, maintain for 1 min after the addition is completed, then raise the temperature to 65°C, maintain an evaporation speed of 200 rpm, stop evaporation when the liquid evaporates to only half, cool to room temperature and filter to obtain 5-iodouridine coated with fluororubber F2311 granules.

[0136] The 5-iodouridine in this example was not granulated.

[0137] Embodiment 29

[0138] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference from Example 28 is that the rotation speed of the fluororubber F2311 solution during dropwise addition in step 2 is 200 rpm, the evaporation speed is 250 rpm, and the method parameters of the remaining steps are the same as those of Example 30.

[0139] The 5-iodouridine in this example granulated and had moderate particle size.

[0140] Embodiment 30

[0141] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference from Example 28 is that the rotation speed of the fluororubber F2311 solution during dropwise addition in step 2 is 300 rpm, the evaporation speed is 350 rpm, and the method parameters of the remaining steps are the same as those of Example 30.

[0142] The 5-iodouridine in this example was granulated, but the particle size was relatively large.

[0143] Embodiment 31

[0144] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference from Example 28 is that the rotation speed of the fluororubber F2311 solution during dropwise addition in step 2 is 400 rpm, the evaporation speed is 450 rpm, and the method parameters of the remaining steps are the same as those of Example 30.

[0145] The 5-iodouridine in this example was not granulated.

[0146] Embodiment 32

[0147] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference from Example 28 is that the rotation speed of the fluororubber F2311 solution during dropwise addition in step 2 is 500 rpm, the evaporation speed is 550 rpm, and the method parameters of the remaining steps are the same as those of Example 30.

[0148] The 5-iodouridine in this example was not granulated.

[0149] Through the comparison of Examples 28 to 32, it was found that the product of the suction filtration method was very different from the product of the solvent evaporation method, and the product could not be granulated at all in the suction filtration method according to the optimal rotation speed of the solvent evaporation method. The product of the group with both the addition speed and the evaporation speed exceeding 400rpm was basically not granulated. This is because if the rotation speed when evaporating the solvent is not fast enough, the fluororubber will sink to the bottom and cannot wrap 5-iodouridine. However, the solvent was not evaporated during the suction filtration process, and the rotation speed was too fast, resulting in the fluororubber being too dispersed and difficult to coat on the 5-iodouridine. However, the rotation speed in Example 28 was too slow, resulting in large pieces of unseparated fluororubber in the product. Examples 29 and 30 were successfully coated. By comparison, Example 29 had a better effect, and the optimal rotation speed was determined to be between 200 and 300rpm.

[0150] Embodiment 33

[0151] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference from Example 28 is that the initial temperature for adding the fluororubber F2311 solution in step 2 is 40°C, the evaporation temperature is 50°C, and the method parameters of the remaining steps are the same as those of Example 30.

[0152] The 5-iodouridine granulation effect in this example was poor, and many of them were not coated with fluororubber F2311.

[0153] Embodiment 34

[0154] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference from Example 28 is that the initial temperature of the dripping of the fluororubber F2311 solution in step 2 is 45°C, the evaporation temperature is 55°C, and the method parameters of the remaining steps are the same as those of Example 30.

[0155] The 5-iodouridine granulation effect in this example was poor, and many of them were not coated with fluororubber F2311.

[0156] Embodiment 35

[0157] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference from Example 28 is that the initial temperature for adding the fluororubber F2311 solution in step 2 is 50°C, the evaporation temperature is 60°C, and the method parameters of the remaining steps are the same as those of Example 30.

[0158] The granulation effect of 5-iodouridine in this embodiment is average, and there is still 5-iodouridine that is not coated with fluororubber F2311.

[0159] By comparing Example 28, Example 33, Example 34 and Example 35, it is found that, similar to the method of evaporating the solvent, the best effect is achieved when the temperature is 55°C-65°C. If the temperature is too low, the evaporation rate will be insufficient and the fluororubber F2311 will not be able to be coated on the 5-iodouridine.

[0160] Embodiment 36

[0161] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference from Example 29 is that the amount of 5-iodouridine used is 0.95 g, the mass of ethanol is 9.5 g, and the method parameters of the remaining steps are the same as those of Example 31.

[0162] The granulation effect of 5-iodouridine in this example is not good, and basically no granulation is formed.

[0163] Embodiment 37

[0164] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference from Example 29 is that the amount of 5-iodouridine used is 0.95 g, the mass of ethanol is 12.35 g, and the method parameters of the remaining steps are the same as those of Example 31.

[0165] Among them, the SEM images of 5-iodouridine without fluororubber F2311 coating and granulation in the particle size range of 2μm, 10μm and 20μm are as follows: Figure 1 , Figure 2 and Figure 3As shown in the figure, it can be seen that the appearance of 5-iodouridine is a columnar polyhedron structure, the smallest particle length is about 10μm, the crystal surface is smooth, the shape is relatively regular, and the crystal defects are few. When the electron microscope range is enlarged, it can be found that the crystals of 5-iodouridine are stacked and scattered irregularly.

[0166] The 5-iodouridine in this example is granulated and has a moderate particle size, and has the best effect.

[0167] The SEM images of 5-iodouridine granulated by fluororubber F2311 in this embodiment in the particle size range of 10 μm, 20 μm and 100 μm are as follows: Figure 4 , Figure 5 and Figure 6 As shown in the figure, it can be seen that Figure 1-Figure 3 The columnar polyhedral 5-iodouridine crystals dispersed in the granulation experiment were bonded together by fluororubber F2311 to form a large mass of 5-iodouridine crystals, and their particle size was significantly reduced. Its uniformity has also improved a lot. The small crystals that were originally scattered have aggregated into large crystals, and its uniformity has also been optimized to form a large mass of 5-iodouridine crystals. This shows the success of granulation. The 5-iodouridine crystals were successfully bonded and coated by fluororubber F2311.

[0168] Depend on Figure 7 It can be seen that the diffraction peaks of 5-iodouridine after coating are at 634 cm -1 752cm -1 1041cm -1 1273cm -1 1431cm -1 1697cm -1 3512cm -1 The diffraction peaks of 5-iodouridine are at 632 cm -1 752cm -1 1041cm -1 1274cm -1 1429cm -1 1691cm -1 3514cm -1 It was found that the diffraction peak positions between the two were basically the same, which shows that the coating process is only a physical process and the chemical process has not changed.

[0169] Depend on Figure 8It can be seen that compared with the raw material 5-iodouridine, the diffraction angle of the product after successful coating and granulation is much higher, which shows that the product has undergone structural changes compared with 5-iodouridine. Through the electron microscope, it can be seen that after coating, many 5-iodouridine crystals are aggregated together. Because they are bonded together, their structure becomes more complex, and the diffraction angle of X-rays naturally becomes more.

[0170] Embodiment 38

[0171] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference from Example 29 is that the amount of 5-iodouridine used is 0.95 g, the mass of ethanol is 16.15 g, and the method parameters of the remaining steps are the same as those of Example 31.

[0172] The 5-iodouridine in this example was granulated but the particles were relatively large.

[0173] Embodiment 39

[0174] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference from Example 29 is that the amount of 5-iodouridine used is 0.95 g, the mass of ethanol is 18.05 g, and the method parameters of the remaining steps are the same as those of Example 31.

[0175] The 5-iodouridine in this example was not granulated.

[0176] Embodiment 40

[0177] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference from Example 29 is that the amount of 5-iodouridine used is 0.95 g, the mass of ethanol is 19 g, and the method parameters of the remaining steps are the same as those of Example 31.

[0178] The 5-iodouridine in this example was not granulated.

[0179] By comparing Example 29 and Example 36-Example 40, the coating effect of the mass ratio of 5-iodouridine to ethanol in Example 37 is the best. When the solvent is too much, the evaporation rate will be affected, thereby affecting the coating effect. Too little solvent will cause the fluororubber to sink to the bottom quickly. Therefore, the mass ratio of 5-iodouridine to ethanol is 1:13, which is the best mass ratio.

[0180] Embodiment 41

[0181] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference from Example 29 is that the amount of fluororubber F2311 used is 0.05 g, the amount of acetone used is 2.45 g, and the method parameters of the remaining steps are the same as those of Example 31.

[0182] The 5-iodouridine in this example was substantially not granulated.

[0183] Embodiment 42

[0184] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference from Example 29 is that the amount of fluororubber F2311 used is 0.05 g, the amount of acetone used is 1.62 g, and the method parameters of the remaining steps are the same as those of Example 31.

[0185] 5-Iodouridine in this example was granulated but many were still not granulated.

[0186] Embodiment 43

[0187] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference from Example 29 is that the amount of fluororubber F2311 used is 0.05 g, the amount of acetone used is 1.2 g, and the method parameters of the remaining steps are the same as those of Example 31.

[0188] The 5-iodouridine in this example is granulated and has moderate granularity, and has a better granular feel than that in Example 42.

[0189] By comparing Example 29 and Example 41-Example 43, it was found that, similar to the method of evaporating the solvent, the coating effect was best when the mass ratio of fluororubber F2311 to acetone was 5:95.

[0190] By comparison of the above embodiments, the product coating effect is the best when the suction filtration method is finally used and the conditions are that the mass ratio of 5-iodouridine to fluororubber F2311 is 95:5, the addition speed is 200 rpm, and the evaporation speed is 250 rpm; the addition temperature is 55°C, the evaporation temperature is 65°C, the mass ratio of 5-iodouridine to ethanol is 1:13, the mass ratio of fluororubber F2311 to acetone is 5:95, and the dripping speed of the fluororubber F2311 solution is 0.8 mL / s.

[0191] Embodiment 44

[0192] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference between this embodiment and embodiment 37 is that the fluororubber F2311 used in step 2 is replaced by modified fluororubber F2311, and the process methods of the remaining steps are the same as those of embodiment 37; wherein the preparation method of modified fluororubber F2311 includes:

[0193] S1. Add 5 g of sodium trifluoromethanesulfonate to 500 mL of deionized water, and stir at 1200 rpm for 2 h to obtain an emulsified system;

[0194] S2, add the emulsified system into the reactor, and evacuate the reactor to 1.2×10 -2 Pa, the emulsified system was heated to 60 ° C, and then 0.5 mol of vinylidene fluoride and 0.5 mol of chlorotrifluoroethylene were added to the emulsified system, and 4 g of potassium persulfate, 2 g of sodium bisulfite and 10 g of maleic anhydride were added in batches while stirring and mixing, and the pressure was increased to 3.6 MPa, and the temperature was raised to 90 ° C to carry out polymerization reaction. After the reaction for 8 hours, the pressure was released and the system was cooled to 4 ° C to obtain fluororubber F2311;

[0195] S3, using Ar plasma to modify the prepared fluororubber F2311, the specific method includes:

[0196] The fluororubber F2311 was cut into thin sheets with a thickness of 0.1 mm and a length and width of 10 cm. The thin sheets were washed with deionized water and placed in a vacuum chamber with a degree of vacuum of 2.2 × 10 -6 Pa, Ar gas is introduced into the vacuum chamber, the flow rate of Ar gas is 15sccm, the radio frequency frequency is 60MHz, the voltage is 500V, Ar plasma directly acts on the thin film to modify the thin film, the modification treatment time is 1 to 3h, and the thin film is taken out and crushed to obtain modified fluororubber F2311.

[0197] Embodiment 45

[0198] This embodiment provides a method for granulating 5-iodouridine using fluororubber F2311. The difference between this embodiment and embodiment 37 is that the fluororubber F2311 used in step 2 is replaced by modified fluororubber F2311, and the process methods of the remaining steps are the same as those of embodiment 37; wherein the preparation method of modified fluororubber F2311 includes:

[0199] S1. Add 10 g of triphenylsulfonium perfluorobutanesulfonate to 800 mL of deionized water, and stir at 2400 rpm for 3 h to obtain an emulsified system;

[0200] S2, add the emulsified system into the reactor, and evacuate the reactor to 1.2×10 -2 Pa, the emulsified system was heated to 70 ° C, and then 0.5 mol of vinylidene fluoride and 0.5 mol of chlorotrifluoroethylene were added to the emulsified system, and 8 g of oxidant, 3 g of reducing agent and 15 g of maleic anhydride were added in batches while stirring and mixing, and the pressure was increased to 3.0 MPa, and the temperature was raised to 90 ° C to carry out polymerization reaction. After the reaction for 8 hours, the pressure was released and the system was cooled to 4 ° C to obtain fluororubber F2311;

[0201] S3, using Ar plasma to modify the prepared fluororubber F2311, the specific method includes:

[0202] The fluororubber F2311 was cut into thin sheets with a thickness of 0.1 mm and a length and width of 10 cm. The thin sheets were washed with deionized water and placed in a vacuum chamber with a degree of vacuum of 1.8 × 10 -6 Pa, Ar gas is introduced into the vacuum chamber, the flow rate of Ar gas is 18 sccm, the radio frequency frequency is 80 MHz, the voltage is 600 V, and Ar plasma directly acts on the thin film to modify the thin film. The modification treatment time is 3 hours. After taking out, the thin film is crushed to obtain modified fluororubber F2311.

[0203] The particle sizes of the 5-iodouridine samples after coating and granulation in Example 1, Example 37, Example 44 and Example 45 and the 5-iodouridine samples not coated and granulated were measured respectively, and the following table was obtained:

[0204]

[0205]

[0206] As can be seen from the above table, Example 1 and Example 37 are the embodiments with the best 5-iodouridine coating and granulation effects in the evaporation method and the suction filtration method, respectively. The particle sizes of the 5-iodouridine after coating and granulation are concentrated in 48.03-233.96 μm and 33.81-179.54 μm, respectively. After Example 44 and Example 45 coated and granulated 5-iodouridine with modified fluororubber, the particle size and distribution of 5-iodouridine were concentrated in 20.42-109.02 μm and 22.60-118.63 μm, respectively. The particle size of 5-iodouridine was significantly reduced, and the particle size distribution was more concentrated, which was not only better than the raw material 5-iodouridine of uncoated granulation, but also better than the 5-iodouridine coated and granulated in Example 1 and Example 37.

[0207] At the same time, in order to measure the flow properties of the uncoated granulated raw material 5-iodouridine, Example 1, Example 37, Example 44 and Example 45 coated granulated 5-iodouridine, the repose angle of 5-iodouridine was measured according to GB / T11986-1989 standard, and the following table was obtained:

[0208] Example 1 Embodiment 37 Embodiment 44 Embodiment 45 Uncoated granulation Angle of repose 40.2 38.5° 33.8° 34.7° 46.3°

[0209] As can be seen from the above table, the repose angle of 5-iodouridine without coating and granulation is 46.3°, while the repose angle of 5-iodouridine after coating and granulation with fluororubber F2311 can be reduced to 40.2° and 38.5°, indicating that after coating and granulation with fluororubber F2311, the flowability of 5-iodouridine has been significantly improved; the repose angle of 5-iodouridine coated and granulated with modified fluororubber F2311 can be further reduced to 33.8° and 34.7°, indicating that the flowability of 5-iodouridine coated and granulated with modified fluororubber F2311 is significantly better than that of 5-iodouridine coated and granulated with fluororubber F2311.

[0210] The number of devices and processing scales described here are used to simplify the description of the present invention. Applications, modifications and variations of the present invention will be obvious to those skilled in the art.

[0211] Although the embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the specification and the implementation modes, and they can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to the specific details and the illustrations shown and described herein.

Claims

1. A method for granulating 5-iodouridine using fluororubber F2311, characterized in that: The following steps are involved: Step 1: prepare 5-iodouridine suspension, and use fluororubber F2311 to prepare fluororubber F2311 solution; Step 2: Add the fluororubber F2311 solution to the 5-iodouridine suspension at a certain rotation speed and a certain dropping speed, maintain the solution for a certain time after the addition is completed, then increase the temperature, maintain a certain rotation speed, evaporate the solvent, and prepare 5-iodouridine coated with fluororubber F2311 granules.

2. The method for granulating 5-iodouridine using fluororubber F2311 as claimed in claim 1, characterized in that: In the step 1, the method for preparing the 5-iodouridine suspension includes: placing 5-iodouridine in ethanol, ultrasonicating for 2 to 10 minutes, and then stirring at an initial temperature of 40° C. to 55° C. and a speed of 200 to 500 rpm for 5 to 15 minutes to obtain a uniform 5-iodouridine suspension; wherein the mass ratio of 5-iodouridine to ethanol is 1:8 to 20.

3. The method for granulating 5-iodouridine using fluororubber F2311 as claimed in claim 1, characterized in that: In the step 1, the fluororubber F2311 is a copolymer of chlorotrifluoroethylene and chloroethylene trifluoride.

4. The method for granulating 5-iodouridine using fluororubber F2311 as claimed in claim 3, characterized in that: In the step 1, the method of using fluororubber F2311 to prepare a fluororubber F2311 solution includes: dissolving fluororubber F2311 in ethyl acetate, wherein the mass ratio of fluororubber F2311 to ethyl acetate is 2-5:95-98, and the mass ratio of 5-iodouridine to fluororubber F2311 is 94-97:3-6.

5. The method for granulating 5-iodouridine using fluororubber F2311 as claimed in claim 1, characterized in that: In the step 2, the rotation speed of dropping the fluororubber F2311 solution is 200-600 rpm, the dropping temperature is 40-60° C., the evaporation rotation speed is 300-500 rpm, and the evaporation temperature is 50-65° C.

6. The method for granulating 5-iodouridine using fluororubber F2311 as claimed in claim 4, characterized in that: The dropping speed of the fluororubber F2311 solution is 0.3-0.9 mL / s.

7. The method for granulating 5-iodouridine using fluororubber F2311 as claimed in claim 1, characterized in that: The step 1 and the step 2 are replaced by: placing 5-iodouridine in a certain proportion of ethanol, ultrasonicating for 2 to 10 minutes, and then granulating at a certain temperature at 300 to 600 rpm for 5 to 15 minutes; raising the temperature to a certain temperature, adding a fluororubber F2311 solution at a certain speed and a certain dropping speed, maintaining the solution for 1 to 3 minutes after the addition is completed, then raising the temperature and changing the speed for evaporation, stopping the evaporation when only half of the liquid has evaporated, cooling to room temperature, and filtering to obtain 5-iodouridine coated with fluororubber F2311 granules.

8. The method for granulating 5-iodouridine using fluororubber F2311 as claimed in claim 7, characterized in that: The rotation speed of dropping the fluororubber F2311 solution is 150-500 rpm, and the dropping temperature is 40-55° C.; the evaporation rotation speed is 200-550 rpm, and the evaporation temperature is 50-65° C.

9. The method for granulating 5-iodouridine using fluororubber F2311 as claimed in claim 7, characterized in that: The solvent of the fluororubber F2311 solution is acetone, and the mass ratio of the fluororubber F2311 to acetone is 2-5:95-98.

10. The method for granulating 5-iodouridine using fluororubber F2311 as claimed in claim 7, characterized in that: The mass ratio of 5-iodouridine to ethanol is 1:10-20: the mass ratio of 5-iodouridine to fluororubber F2311 is 94-97:3-6.

Images