Synthesis and preparation process of ultrahigh polyphosphoric acid compound
By adding phosphorus pentoxide and gradient catalysts in stages, the problems of low molecular weight and insufficient thermal stability in the traditional synthesis of ultra-high polyphosphate compounds were solved, and the preparation of ultra-high polyphosphate compounds with high molecular weight and high thermal stability was achieved.
Patent Information
- Application Number
- CN202511085048.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-04
- Publication Date
- 2025-11-14
AI Technical Summary
In existing processes for synthesizing ultra-high polyphosphate compounds, traditional single catalyst systems are prone to premature chain termination reactions, making it difficult to break through the 5000 molecular weight limit, limiting phosphorus content, and resulting in insufficient thermal stability.
A gradient addition method was adopted, in which phosphorus pentoxide was added in five stages and different types of catalysts were added in three stages. By combining the synergistic effect of palladium-platinum-based, polyol and sugar derivative catalysts, the reaction rate and temperature were controlled to gradually improve the reaction activity and molecular weight distribution.
It achieves precise control of molecular weight in the range of 500 to 35,000, significantly improves phosphorus content and thermal stability, avoids premature chain termination, and the hydrolysis rate of the product is less than 5% after three years of storage at room temperature.
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Figure CN120943221A_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of inorganic polymer synthesis technology, and more specifically, to a synthesis and preparation process for an ultra-high polyphosphate compound. Background Technology
[0002] Phosphoric acid compounds are a class of functional materials with phosphorus-oxygen bonds as their core structure, and are widely used in new energy, biomedicine, flame retardant materials, and metal surface treatment. Among them, high molecular weight polyphosphoric acid compounds, due to their unique phosphorus enrichment characteristics and thermal stability, have shown irreplaceable application value in high-end fields such as solid-state battery electrolytes, biological tissue repair, and heavy metal adsorption. However, traditional phosphate-based biomaterials, due to their low molecular weight and easy hydrolysis, have always been unable to meet complex clinical needs.
[0003] The existing synthesis processes for ultra-high polyphosphate compounds have the following problems: traditional single catalyst systems are prone to premature chain termination reactions during polymerization, making it difficult to break through the molecular weight of the product, which is usually below 5000. The phosphorus content is limited, resulting in insufficient thermal stability. Summary of the Invention
[0004] To address the issues of low molecular weight, easy hydrolysis, and insufficient thermal stability of phosphate compounds in existing technologies, this application provides a synthesis and preparation process for ultra-high polyphosphate compounds.
[0005] The synthesis and preparation process of an ultra-high polyphosphate compound provided in this application adopts the following technical solution:
[0006] A process for synthesizing and preparing an ultra-high polyphosphate compound includes the following steps:
[0007] S1. Add 29 kg to 62 kg of phosphoric acid to the reactor;
[0008] S2. Add 7-28 kg of the first portion of phosphorus pentoxide and heat to 80-135°C.
[0009] S3. Add 0.5 kg to 6 kg of the first catalyst and stir the reaction at 80°C to 150°C for 2 to 12 hours.
[0010] S4. Add 7-28 kg of the second part of phosphorus pentoxide and stir the reaction at 80℃-160℃ for 2-15 hours.
[0011] S5. Add 0.3 kg to 6 kg of the second catalyst and stir the reaction at 80°C to 180°C for 2 to 15 hours.
[0012] S6. Add 7-28 kg of the third part of phosphorus pentoxide and stir the reaction at 80℃-180℃ for 2-15 hours.
[0013] S7. Add 0.3 kg to 6 kg of the third catalyst and stir the reaction at 80°C to 180°C for 2 to 15 hours.
[0014] S8. Add 7-28 kg of the fourth part of phosphorus pentoxide and stir the reaction at 80℃-220℃ for 2-18 hours.
[0015] S9. Add 7-28 kg of the fifth part of phosphorus pentoxide and stir the reaction at 80℃-250℃ for 2-24 hours.
[0016] S10. Add 100kg to 260kg of pure water and stir for 2 to 6 hours.
[0017] S11. Add 1kg to 10kg of activated carbon and stir for 2 hours;
[0018] S12, Filter and package the product.
[0019] By adopting the above technical solution, the addition of phosphorus pentoxide to the reactor in five stages, with each addition controlled at 7kg to 28kg, achieves gradual polymerization and controls the reaction rate, thereby achieving a uniform molecular weight distribution. Controlling different reaction temperatures at different stages gradually increases reaction activity and promotes the polymerization reaction, thus improving thermal stability. Adding different amounts of catalyst in four stages precisely regulates the polymerization process and optimizes molecular weight distribution, thereby increasing product viscosity. The gradient-stage catalyst system, using palladium-platinum based, polyol, and sugar derivative catalysts at different stages to form a synergistic catalytic effect, achieves 5 Precise control of the molecular weight range from 0 to 35,000 is achieved, with the 25,000-35,000 high-polymer segment suitable for the biomedical field, the 5,000-15,000 medium-polymer segment suitable for flame retardants, and the 500-5,000 low-polymer segment meeting the requirements of solid-state batteries. This results in a significant improvement in the phosphorus content of the polymer and the thermal stability of the product, with a hydrolysis rate of <5% after three years of storage at room temperature. It also effectively avoids the problem of premature chain termination during polymerization. The total added mass of phosphoric acid is 6.5% to 18.5% of the total mass of the reaction system, the total added mass of phosphorus pentoxide (phosphorus pentoxide) five times accounts for 25% to 38% of the total mass of the reaction system, the total added mass of catalyst is 1% to 5% of the total mass of the reaction system, and the total added mass of pure water is 1% to 5% of the total mass of the reaction system.
[0020] Preferably, the phosphorus pentoxide is added in five batches, and the interval between the addition of materials in steps S4, S6, S8, and S9 and the previous addition is at least 2 hours.
[0021] By adopting the above technical solution, phosphorus pentoxide is added in stages during steps S4, S6, S8, and S9, with each addition spaced at least 2 hours apart from the previous one. This method of adding phosphorus pentoxide in stages avoids the violent exothermic reaction and excessively fast reaction rate caused by adding a large amount of phosphorus pentoxide at once, thereby preventing the reaction from getting out of control and the equipment from overpressure.
[0022] Preferably, the catalyst is added in three stages, with the addition points located at steps S3, S5, and S7, and each catalyst addition operation is located between two consecutive phosphorus pentoxide addition operations.
[0023] By adopting the above technical solution, the catalyst is added in stages in steps S3, S5, and S7, which plays a role in precisely controlling the polymerization reaction process. Each addition of catalyst occurs between two additions of phosphorus pentoxide, which ensures that the catalyst is evenly distributed during the continuous addition of phosphorus pentoxide, thereby improving the polymerization reaction efficiency and controlling the reaction rate.
[0024] Preferably, the catalyst is selected from at least one of palladium-based catalysts, platinum-based catalysts, polyol catalysts, and carbohydrate derivative catalysts.
[0025] By adopting the above technical solutions, the selection of palladium-based or platinum-based catalysts improves reaction selectivity. Polyol catalysts and sugar derivative catalysts, due to the presence of multiple active hydroxyl groups in their structures, can provide multiple reaction sites, thereby enhancing reaction activity. Such multi-active-site catalysts help to increase the reaction rate, thus achieving the effect of shortening reaction time and improving production efficiency.
[0026] Preferably, the palladium-based catalyst is palladium chloride or palladium on carbon; the platinum-based catalyst is chloroplatinic acid or platinum black; the polyol catalyst is selected from propylene glycol, glycerol, n-butanol, pentaerythritol, and inositol; and the sugar derivative catalyst is selected from oligosaccharides and chitosan.
[0027] By adopting the above technical solutions, palladium-based catalysts can significantly increase the reaction rate of phosphorus pentoxide and phosphoric acid while reducing the formation of by-products, thereby improving product purity and reaction efficiency; platinum-based catalysts help form more uniform polymers in the polymerization reaction, improving the thermal stability and mechanical properties of the product, thus improving product performance; polyol catalysts can increase the rate and depth of the polymerization reaction, improve the molecular weight distribution and mechanical strength of the product, thus improving the application performance of the product; and sugar derivative catalysts can enhance the product's resistance to hydrolysis and thermal stability, improve the product's biodegradability, thus improving the product's environmental friendliness.
[0028] Preferably, the catalysts added in steps S3, S5, and S7 are of different types, wherein: step S3 uses a palladium-based or platinum-based catalyst; step S5 uses a polyol catalyst; and step S7 uses a sugar derivative catalyst.
[0029] By adopting the above technical solutions, the use of palladium-based or platinum-based catalysts can promote the initial reaction between phosphorus pentoxide and phosphoric acid, thereby rapidly initiating the polymerization reaction and increasing the reaction rate. The use of polyol catalysts in the middle stage of the polymerization reaction can further promote the polymerization process, increase the molecular weight and mechanical strength of the product, and improve its physical properties. Sugar derivative catalysts, due to the presence of multiple hydroxyl and carbonyl groups in their structure, can form stable intermediates with phosphoric acid and phosphorus pentoxide, thus promoting the polymerization reaction and improving product stability.
[0030] Preferably, in step S9, after the temperature is raised to 200℃~250℃, the stirring speed is controlled to be 100~300rpm.
[0031] By adopting the above technical solution, the appropriate high temperature can promote the further reaction between phosphorus pentoxide and phosphoric acid, accelerate the polymerization process, and help improve the thermal stability and molecular weight of the product. Controlling the stirring speed within the range of 100 to 300 rpm can ensure the uniform mixing of materials in the reactor and avoid local overheating or uneven reaction.
[0032] Preferably, the system temperature is ≤50℃ when the activated carbon is added in step S11, and the activated carbon is industrial grade or food grade.
[0033] By adopting the above technical solution, the system temperature is controlled to not exceed 50℃ when activated carbon is added, which can prevent changes in the physical or chemical properties of activated carbon due to high temperature, maintain its adsorption performance, and select industrial-grade or food-grade activated carbon according to the needs of different application scenarios to ensure the safety and compliance of the product.
[0034] Preferably, in step S12, a filter membrane with a pore size of 0.1 to 5 μm is used for filtration.
[0035] By adopting the above technical solution, the use of a smaller pore size can avoid damaging polymer molecules during the filtration process and maintain the integrity of their molecular structure.
[0036] Preferably, before adding phosphorus pentoxide in steps S4, S6, S8, and S9, the reaction system is cooled to 80°C to 100°C before adding the phosphorus pentoxide.
[0037] By adopting the above technical solution, and by pre-cooling the reaction system to 80℃~100℃, the rapid temperature rise caused by the exothermic reaction during the feeding of phosphorus pentoxide can be avoided, thereby controlling the reaction temperature within a safe and suitable range.
[0038] In summary, this application has the following beneficial effects:
[0039] 1. Because this application adopts a gradient-stage catalyst system, and because palladium-platinum-based, polyol and sugar derivative catalysts are used in different stages to form a synergistic catalytic effect, the effect of significantly improving the phosphorus content of the polymer and the thermal stability of the product is achieved, while effectively avoiding the problem of premature chain termination during the polymerization process.
[0040] 2. The method of this application effectively suppresses the violent boiling caused by the exothermic reaction during the feeding process by adding phosphorus pentoxide in stages and at a low temperature of 80°C to 100°C. Therefore, it achieves the effects of precisely controlling the molecular weight distribution of polymer, significantly reducing the risk of polymer chain breakage, and ensuring the integrity of polymer structure.
[0041] 3. In this application, a gradient heating program containing a specific high-temperature zone is preferably adopted, thereby achieving the core effect of driving full dehydration and polycondensation and efficiently forming the POP main chain structure, which greatly improves the thermal stability and molecular weight of the polymer.
[0042] 4. The method of this application, by selecting a specific type of catalyst and strictly limiting its addition conditions and temperature, effectively avoids the risk of toxic impurities and side reactions that may be introduced by traditional metal oxide catalysts. Attached Figure Description
[0043] Figure 1 This is a flowchart of a synthesis and preparation process for an ultra-high polyphosphate compound provided in this application;
[0044] Figure 2 These are photographs of the polyphosphate compound prepared in Example 1 of this application.
[0045] Figure 3 This is the FTIR spectrum of the polyphosphate compound prepared in Example 1 of this application;
[0046] Figure 4 This is the FTIR matched spectrum of the polyphosphate compound prepared in Example 1 of this application;
[0047] Figure 5 This is the 31P-NMR spectrum of the polyphosphate compound prepared in Example 1 of this application;
[0048] Figure 6 This is a molecular weight distribution curve of the polyphosphate compound prepared in Example 1 of this application;
[0049] Figure 7 This is a molecular weight elution curve of the polyphosphate compound prepared in Example 1 of this application. Detailed Implementation
[0050] The present application will be further described in detail below with reference to the accompanying drawings and embodiments.
[0051] Technical concept:
[0052] In traditional synthesis processes, phosphorus pentoxide is often added to the reaction system all at once. Because its reaction with phosphoric acid is vigorous and exothermic, it can easily lead to a sudden rise in local temperature, resulting in more side reactions, generating too much oligophosphoric acid impurities, and reducing the degree of polymerization and purity of the product. At the same time, the method of adding catalyst is also relatively simple, mostly added all at once, which makes it difficult to achieve the best catalytic effect at different stages of the reaction, resulting in uneven reaction rate, prolonged reaction time, and low production efficiency.
[0053] The technical solution of this application addresses the above-mentioned problems by adopting the following approach: phosphorus pentoxide is added in five stages, with a strict control of the interval between each addition being at least 2 hours. Simultaneously, the reaction system is cooled to 50℃~110℃ before each phosphorus pentoxide addition. This effectively slows down the reaction rate, avoids local overheating, reduces side reactions, and promotes higher polymerization of the product. The catalyst is added in three stages, with each addition occurring between two consecutive phosphorus pentoxide additions. Different types of catalysts, including palladium-based catalysts, platinum-based catalysts, polyol catalysts, and sugar derivative catalysts, are selected and added at different stages of the reaction, ensuring that the catalyst fully exerts its catalytic effect at each stage, accelerating the reaction rate, and shortening the reaction time.
[0054] The raw materials involved in this technical solution, namely phosphoric acid, phosphorus pentoxide, pure water, and activated carbon, are all existing products that can be obtained directly.
[0055] Preparation Example 1
[0056] The preparation steps of platinum-based catalysts are as follows:
[0057] Add 5.2g of chloroplatinic acid hexahydrate (H2PtCl6·6H2O) to a 500ml three-necked flask, add 200ml of deionized water preheated in a 40℃ constant temperature water bath, and start stirring until the crystals are completely dissolved to form a bright yellow transparent solution. Then, use a constant pressure dropping funnel to slowly add 83ml of 20wt% sodium gluconate solution to the system at a rate of 3ml / min. After the addition is complete, adjust the pH to 8.5.
[0058] The reaction system was heated to 75°C and kept under nitrogen protection for 2 hours. During this period, the solution underwent a typical color change: initially bright yellow → turned brownish-red after 30 minutes → transitioned to bluish-gray after 90 minutes → and finally turned into stable Prussian blue after 120 minutes.
[0059] The resulting homogeneous liquid was immediately transferred to a centrifugal spray dryer. The feed rate was set to 3 ml / s, the atomizing disc speed to 15000 rpm, and the inlet air temperature to 180℃. The blue powder product deposited in the dryer was collected and then processed in a vacuum drying oven at 40℃ for 12 hours and passed through a 200-mesh sieve to obtain finished catalyst powder with a particle size of <3 μm.
[0060] This application provides a synthesis and preparation process for ultra-high polyphosphate compounds. The following details the synthesis and preparation process for an ultra-high polyphosphate compound provided in the embodiments of this application.
[0061] Example 1
[0062] This application provides a synthesis and preparation process for ultra-high polyphosphate compounds, including the following steps:
[0063] S1. Add 45.5 kg of phosphoric acid to the reactor;
[0064] S2. Add the first portion of phosphorus pentoxide, 17 kg, and heat to 105℃;
[0065] S3. Add 3 kg of the first catalyst, using chloroplatinic acid as a platinum-based catalyst, and stir the reaction at 115°C for 7 hours.
[0066] S4. First, cool the reaction system to 90°C, then add the second part of phosphorus pentoxide 17kg, with an interval of 2 hours between the first and second additions, and stir the reaction at 120°C for 8.5 hours.
[0067] S5. Add the second 3 kg of catalyst, using pentaerythritol as a polyol catalyst, and stir the reaction at 130°C for 8.5 hours.
[0068] S6. First, cool the reaction system to 90°C, then add the third part of phosphorus pentoxide 17kg, with an interval of 2 hours between the previous addition, and stir the reaction at 130°C for 8.5 hours.
[0069] S7. Add the third part of catalyst 3kg, using oligosaccharide and sugar derivative catalyst, and stir the reaction at 130℃ for 8.5 hours.
[0070] S8. First, cool the reaction system to 90°C, then add the fourth part of phosphorus pentoxide 17kg, with an interval of 2 hours between the previous addition, and stir the reaction at 150°C for 10 hours.
[0071] S9. First, cool the reaction system to 90°C, then add the fifth part of phosphorus pentoxide 17kg, with an interval of 2 hours between the previous addition. After heating to 225°C, control the stirring speed to 200rpm and stir the reaction at this temperature for 13 hours.
[0072] S10. Add 180kg of pure water and stir for 4 hours.
[0073] S11. Add 5.5 kg of activated carbon, control the system temperature at 50℃, and stir for 2 hours.
[0074] S12. Filter using a 2.5μm pore size filter membrane and dispense the product.
[0075] Example 2
[0076] This application provides a synthesis and preparation process for ultra-high polyphosphate compounds, including the following steps:
[0077] S1. Add 29 kg of phosphoric acid to the reactor;
[0078] S2. Add the first 7 kg of phosphorus pentoxide and heat to 80°C;
[0079] S3. Add the first part of catalyst 0.5 kg, which is palladium on carbon and is a palladium-based catalyst, and stir the reaction at 80°C for 2 hours.
[0080] S4. First, cool the reaction system to 80°C, then add the second part of phosphorus pentoxide 7kg, with an interval of 2 hours between the previous addition and the previous addition. Stir the reaction at 80°C for 2 hours.
[0081] S5. Add the second catalyst, 0.3 kg, using propylene glycol as a polyol catalyst, and stir the reaction at 80°C for 2 hours.
[0082] S6. First, cool the reaction system to 80°C, then add the third part of phosphorus pentoxide 7kg, with an interval of 2 hours between the previous addition and the previous addition. Stir the reaction at 80°C for 2 hours.
[0083] S7. Add the third catalyst, 0.3 kg, using oligosaccharide and sugar derivative catalyst, and stir the reaction at 80°C for 2 hours.
[0084] S8. First, cool the reaction system to 80°C, then add the fourth part of phosphorus pentoxide 7kg, with an interval of 2 hours between the previous addition and the previous addition. Stir the reaction at 80°C for 2 hours.
[0085] S9. First, cool the reaction system to 80°C, then add the fifth part of phosphorus pentoxide 7kg, with an interval of 2 hours between the previous addition. After heating to 200°C, control the stirring speed to 100rpm and stir the reaction at this temperature for 2 hours.
[0086] S10. Add 100kg of pure water and stir for 2 hours;
[0087] S11. Add 1 kg of activated carbon, control the system temperature at 40℃, and stir for 2 hours. The activated carbon is food grade.
[0088] S12. Filter using a 0.1μm pore size filter membrane and dispense the product.
[0089] Example 3
[0090] This application provides a synthesis and preparation process for ultra-high polyphosphate compounds, including the following steps:
[0091] S1. Add 62 kg of phosphoric acid to the reactor;
[0092] S2. Add the first portion of phosphorus pentoxide, 28 kg, and heat to 135℃;
[0093] S3. Add 6 kg of the first catalyst, using palladium chloride as the catalyst, and stir the reaction at 150°C for 12 hours.
[0094] S4. First, cool the reaction system to 100℃, then add the second part of phosphorus pentoxide 28kg, with an interval of 3 hours between the previous addition, and stir the reaction at 160℃ for 15 hours.
[0095] S5. Add the second 6 kg of catalyst, using inositol as a polyol catalyst, and stir the reaction at 180°C for 15 hours.
[0096] S6. First, cool the reaction system to 100℃, then add the third part of phosphorus pentoxide 28kg, with an interval of 3 hours between the previous addition, and stir the reaction at 180℃ for 15 hours.
[0097] S7. Add the third part of catalyst 6kg, using chitosan as a sugar derivative catalyst, and stir the reaction at 180℃ for 15 hours.
[0098] S8. First, cool the reaction system to 100℃, then add the fourth part of phosphorus pentoxide 28kg, with an interval of 3 hours between the previous addition, and stir the reaction at 220℃ for 18 hours.
[0099] S9. First, cool the reaction system to 100℃, then add the fifth part of phosphorus pentoxide 28kg, with an interval of 3 hours between the previous addition. After heating to 250℃, control the stirring speed to 300rpm and stir the reaction at this temperature for 24 hours.
[0100] S10. Add 260 kg of pure water and stir for 6 hours.
[0101] S11. Add 10 kg of activated carbon, control the system temperature at 50℃, and stir for 2 hours.
[0102] S12. Filter using a 5μm pore size filter membrane and dispense the product.
[0103] Comparative Example 1
[0104] A synthesis and preparation process for an ultra-high polyphosphate compound, the steps of which differ from those in Example 1 only in that all catalysts are replaced with a single pentaerythritol, and the total mass is the same as that in Example 1, which is 9 kg.
[0105] The only difference between the steps is that pentaerythritol catalyst is added uniformly in steps S3, S5 and S7, 3 kg at a time.
[0106] Comparative Example 2
[0107] A synthesis and preparation process for an ultra-high polyphosphate compound, the only difference from Example 1 is that the constant temperature of 100°C is maintained throughout the process, and the heating procedure in Example 1 is cancelled.
[0108] The only difference between the steps is that in S2, the temperature is not changed after it is raised to 100℃; in S9, the 225℃ high-temperature section is removed, and the reaction is maintained at 100℃ for 13 hours.
[0109] Comparative Example 3
[0110] A synthesis and preparation process for an ultra-high polyphosphate compound, the only difference from Example 1 is that phosphorus pentoxide is added in step S2 in one step, with a total amount the same as in Example 1;
[0111] The only difference between the steps is that the phosphorus pentoxide addition step is removed in steps S4, S6, S8, and S9; and the reaction time in steps S3-S7 is reduced to 2 hours per step.
[0112] Comparative Example 4
[0113] A synthesis and preparation process for an ultra-high polyphosphate compound, the steps of which differ from those in Example 1 only in that the catalyst is replaced with conventional nickel sulfate and zinc oxide, with a total mass of 9 kg;
[0114] The only difference between the steps is that 4.78 kg of nickel sulfate is added in step S3; 4.77 kg of zinc oxide is added in step S5; and no catalyst is added in step S7.
[0115] The performance test results of Examples 1-3 and Comparative Examples 1-4 are shown in Table 1.
[0116] Table 1:
[0117] project Phosphorus content thermal stability Viscosity Example 1 13.57％ 285℃ 1520cP Example 2 12.06％ 258℃ 1410cP Example 3 12.94％ 265℃ 1430cP Comparative Example 1 10.25％ 210℃ 680cP Comparative Example 2 8.95％ 172℃ 380cP Comparative Example 3 10.68％ 235℃ 420cP Comparative Example 4 11.73％ 190℃ 850cP
[0118] Note:
[0119] Phosphorus content testing standards:
[0120] GB / T1871.2-2022 Determination of phosphorus pentoxide content in phosphate rock and phosphate concentrate by gravimetric method of quinoline phosphomolybdate.
[0121] Thermal stability testing standards:
[0122] GB / T2918-2018 Plastics Thermogravimetric Analysis (TGA) - Determination of Decomposition Temperature.
[0123] Viscosity testing standards:
[0124] GB / T22235-2020 Determination of viscosity of liquids - Rotational viscometer method.
[0125] Based on Examples 1-3 and Comparative Example 1, and in conjunction with Table 1, it can be seen that the gradient catalyst system has a significant synergistic effect on improving phosphorus content and thermal stability, and the multi-element catalytic system can avoid premature chain termination.
[0126] Based on Examples 1-3 and Comparative Example 2, and in conjunction with Table 1, it can be seen that the gradient heating process is the core control element of the dehydration polycondensation process, and the high-temperature section in step S9 can effectively drive the formation of POP bonds.
[0127] Based on Examples 1-3 and Comparative Example 3, and in conjunction with Table 1, it can be seen that the phased feeding of phosphorus pentoxide plays a crucial role in regulating the molecular weight distribution. Phased feeding can effectively suppress boiling over and thus reduce chain breakage.
[0128] Combining Examples 1-3 and Comparative Example 4 with Table 1, it can be seen that the specific catalyst system has a significant safety advantage compared with traditional metal oxides, thereby avoiding the introduction of toxic impurities.
[0129] Combined with Example 1 and Appendix Figure 3 and attached Figure 4 It can be seen that: POP bonds are fully formed but residual sulfite impurities remain, 1240cm -1 Strong peak confirms P=O skeleton formation, 900cm -1 The broad peaks show a chain-like polymer structure, in which... Figure 4 The matching substance was anhydrous sodium sulfite, and the matching degree was 74.17%.
[0130] Combined with Example 1 and Appendix Figure 5 It can be seen that the molecular chain length of the product is controllable.
[0131] Combined with Example 1 and Appendix Figure 6It can be seen that the bimodal distribution structure is direct evidence of the staged feeding process, and the coexistence of the two peaks synergistically improves thermal stability and viscosity.
[0132] Combined with Example 1 and Appendix Figure 7 It can be seen that the main peak is symmetrical and has no tail, indicating that there are no degradation products.
[0133] Combined with Example 1 and Appendix Figure 5 , 6 Analysis revealed that the product obtained in Example 1 exhibits an α-helical conformation; this helical structure is formed by the synergistic induction of gradient heating and staged catalysis, which can significantly improve biocompatibility.
[0134] This specific embodiment is merely an explanation of this application and is not intended to limit it. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.
Claims
1. A synthesis and preparation process for an ultra-high polyphosphate compound, characterized in that: Includes the following steps: S1. Add 29 kg to 62 kg of phosphoric acid to the reactor; S2. Add 7-28 kg of the first portion of phosphorus pentoxide and heat to 80-135°C. S3. Add 0.5 kg to 6 kg of the first catalyst and stir the reaction at 80°C to 150°C for 2 to 12 hours. S4. Add 7-28 kg of the second part of phosphorus pentoxide and stir the reaction at 80℃-160℃ for 2-15 hours. S5. Add 0.3 kg to 6 kg of the second catalyst and stir the reaction at 80°C to 180°C for 2 to 15 hours. S6. Add 7-28 kg of the third part of phosphorus pentoxide and stir the reaction at 80℃-180℃ for 2-15 hours. S7. Add 0.3 kg to 6 kg of the third catalyst and stir the reaction at 80°C to 180°C for 2 to 15 hours. S8. Add 7-28 kg of the fourth part of phosphorus pentoxide and stir the reaction at 80℃-220℃ for 2-18 hours. S9. Add 7-28 kg of the fifth part of phosphorus pentoxide and stir the reaction at 80℃-250℃ for 2-24 hours. S10. Add 100kg to 260kg of pure water and stir for 2 to 6 hours. S11. Add 1kg to 10kg of activated carbon and stir for 2 hours; S12, Filter and package the product.
2. The synthesis and preparation process of an ultra-high polyphosphate compound according to claim 1, characterized in that: The phosphorus pentoxide is added in five batches, with an interval of at least 2 hours between each batch in steps S4, S6, S8, and S9.
3. The synthesis and preparation process of an ultra-high polyphosphate compound according to claim 1, characterized in that: The catalyst is added in three stages, with the addition points located at steps S3, S5, and S7, and each catalyst addition operation is located between two consecutive phosphorus pentoxide addition operations.
4. The synthesis and preparation process of an ultra-high polyphosphate compound according to claim 1, characterized in that: The catalyst is selected from at least one of palladium-based catalysts, platinum-based catalysts, polyol catalysts, and carbohydrate derivative catalysts.
5. The synthesis and preparation process of an ultra-high polyphosphate compound according to claim 4, characterized in that: The palladium-based catalyst is palladium chloride or palladium on carbon; the platinum-based catalyst is chloroplatinic acid or platinum black; the polyol catalyst is selected from propylene glycol, glycerol, n-butanol, pentaerythritol, and inositol; the sugar derivative catalyst is selected from oligosaccharides and chitosan.
6. The synthesis and preparation process of an ultra-high polyphosphate compound according to claim 5, characterized in that: The catalysts added in steps S3, S5, and S7 are different from each other. Specifically, step S3 uses a palladium-based or platinum-based catalyst; step S5 uses a polyol catalyst; and step S7 uses a sugar derivative catalyst.
7. The synthesis and preparation process of an ultra-high polyphosphate compound according to claim 1, characterized in that: In step S9, after heating to 200℃~250℃, the stirring speed is controlled at 100~300rpm.
8. The synthesis and preparation process of an ultra-high polyphosphate compound according to claim 1, characterized in that: In step S11, the system temperature is ≤50℃ when activated carbon is added, and the activated carbon is industrial grade or food grade.
9. The synthesis and preparation process of an ultra-high polyphosphate compound according to claim 1, characterized in that: In step S12, a filter membrane with a pore size of 0.1 to 5 μm is used for filtration.
10. The synthesis and preparation process of an ultra-high polyphosphate compound according to claim 1, characterized in that: Before adding phosphorus pentoxide in steps S4, S6, S8, and S9, the reaction system should be cooled to 80℃~100℃ before adding the phosphorus pentoxide.