A method for synthesizing isomeric alcohol phosphonate monoesters
Patent Information
- Application Number
- CN202610730389.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-05-26
- Publication Date
- 2026-09-25
AI Technical Summary
但该路线存在严重的技术缺陷:其一,三氯氧磷属于高危化学品,采购、运输及储存均存在极大风险;其二,反应过程中会释放大量氯化氢(HCl)气体,对生产设备造成极强的腐蚀,需采用昂贵的耐酸蚀特种设备,导致生产成本居高不下
本发明通过引入催化剂及特定量的水参与反应,配合精准的原料摩尔比与过氧化氢水解工艺,在安全环保的前提下,有效克服了传统五氧化二磷法易生成双酯的缺陷,成功实现了磷酸单酯的高选择性合成,确保了产物酯化率及单酯含量同时满足高性能工业应用的标准。
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Abstract
Description
Technical Field
[0001] This invention relates to the field of isomeric alcohol phosphate synthesis technology, specifically a method for synthesizing isomeric alcohol phosphate monoesters. Background Technology
[0002] Isomeric alcohol phosphates, as high-performance anionic surfactants, are widely used in metal processing, pesticide formulations, textile printing and dyeing, and cosmetics due to their unique wetting, emulsifying, and antistatic properties. Monophosphates, with their strong hydrophilicity and high solubility in water, primarily impart excellent emulsifying and wetting properties to products; while diesters, with their stronger lipophilicity, are mainly used in lubricant additives and industrial coatings.
[0003] However, commercially available isomeric alcohol phosphates generally suffer from low monoester content, with the mono- and diester ratio of most products being approximately 1:1, and the monoester content typically below 70%. With the development of industrial technology, high-end metalworking fluids and novel pesticide formulations place higher demands on the emulsification and stability of phosphate esters, urgently requiring products with a monoester content of over 90%, a demand that current processes cannot meet.
[0004] Currently, the industry typically relies on phosphorus oxychloride (POCl3) as a raw material to prepare high-content monophosphate esters. However, this route has serious technical drawbacks: firstly, phosphorus oxychloride is a highly hazardous chemical, posing significant risks during procurement, transportation, and storage; secondly, the reaction process releases large amounts of hydrogen chloride (HCl) gas, causing severe corrosion to production equipment, requiring expensive acid-resistant special equipment, resulting in high production costs. In addition, there are attempts to synthesize directly using phosphorus pentoxide (P2O5), but due to the extremely high reactivity of phosphorus pentoxide, it readily reacts with the two hydroxyl groups of alcohols, leading to excessive phosphate diester byproducts in the product, making it difficult to synthesize high-content monophosphate esters in a targeted manner.
[0005] Therefore, developing a method for the targeted synthesis of isomeric alcohol phosphate monoesters with safe and environmentally friendly raw materials, no special requirements for equipment, and high monoester content (>90%) is a technical problem that urgently needs to be solved in this field. Summary of the Invention
[0006] The purpose of this invention is to provide a method for synthesizing isomeric alcohol phosphate monoesters to solve the problems mentioned in the background art.
[0007] To achieve the above objectives, the embodiments of the present invention provide the following technical solutions: A method for synthesizing an isomeric alcohol phosphate monoester includes the following steps: Add isomeric alcohol, catalyst and water to the reaction vessel, and add phosphorus pentoxide at a controlled temperature of 40-60℃ (to prevent the reaction from being too vigorous). After the addition is complete, raise the temperature to 80-100℃ to carry out the esterification reaction and keep the reaction at this temperature for 3-5 hours (to ensure that the esterification reaction is fully carried out). After the reaction is complete, the temperature is lowered to 70-90℃, and hydrogen peroxide (H2O2) is added for hydrolysis and decolorization treatment to obtain isomeric alcohol phosphate monoester; The molar ratio of the isomeric alcohol to phosphorus pentoxide is 1.7-2.3:1; the amount of catalyst is 0.2%-0.8% of the mass of the isomeric alcohol; the amount of water added is 1%-4% of the mass of the isomeric alcohol; and the amount of hydrogen peroxide added is 1%-3% of the total mass of the materials.
[0008] As a further aspect of the present invention: the molar ratio of the isomeric alcohol to phosphorus pentoxide is 1.9-2.0:1; the amount of catalyst used is 0.5%-0.6% of the mass of the isomeric alcohol; and the amount of water added is 2%-2.5% of the mass of the isomeric alcohol.
[0009] As a further aspect of the present invention, the phosphorus pentoxide is added at a time of 0.5-2 hours.
[0010] As a further aspect of the present invention: the esterification reaction is carried out at a temperature of 85°C for a reaction time of 4 hours.
[0011] As a further aspect of the present invention: the catalyst is selected from at least one of solid catalyst FEC or liquid catalyst AMC; wherein, the FEC is a zirconium oxide modified product, and the AMC is a titanate modified product.
[0012] As a further aspect of the present invention: the catalyst is a liquid catalyst AMC.
[0013] As a further aspect of the present invention: the hydrogen peroxide is added over a period of 0.5-2 hours, and the hydrolysis time is 2-4 hours; the hydrolysis decolorization temperature is 70-90°C.
[0014] As a further aspect of the present invention: the amount of hydrogen peroxide added is 1.25% of the total material mass, the dripping time is 1.5h, the hydrolysis time is 3h, and the hydrolysis temperature is 80℃.
[0015] As a further aspect of the present invention: the addition of water is used to regulate the reaction system, converting phosphorus pentoxide into metaphosphoric acid and / or pyrophosphoric acid, so as to directionally inhibit the formation of phosphate diesters; the hydrogen peroxide not only acts as a decolorizing agent, but also participates in the reaction together with the active oxygen and water generated during its hydrolysis process, inhibiting the excessive hydrolysis of phosphate monoesters and improving the color of the product.
[0016] As a further aspect of the present invention, the product obtained by the method has an esterification rate of greater than 95% and a phosphate monoester content of greater than 90%.
[0017] Compared with the prior art, the beneficial effects of the embodiments of the present invention are: This invention, by introducing a catalyst and a specific amount of water into the reaction, combined with a precise raw material molar ratio and hydrogen peroxide hydrolysis process, effectively overcomes the defect of easy diester formation in the traditional phosphorus pentoxide method under the premise of safety and environmental protection, and successfully achieves highly selective synthesis of phosphate monoesters, ensuring that the esterification rate and monoester content of the product simultaneously meet the standards for high-performance industrial applications.
[0018] Overall, this invention replaces the highly hazardous phosphorus oxychloride with safe and environmentally friendly phosphorus pentoxide, and achieves a highly efficient and green synthesis with an esterification rate of >95% and a monoester content of >90% through the synergistic regulation of catalyst and water. Detailed Implementation
[0019] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0020] Example 1
[0021] 158 g of isomeric decaol, 1.58 g of deionized water, and 0.32 g of solid catalyst FEC (zirconia-modified) were added to a reaction flask. Stirring was started, and the temperature was raised to 40°C. 87 g of phosphorus pentoxide was then added in batches, maintaining the reaction temperature below 60°C, over approximately 2 hours. The temperature was then raised to 100°C and maintained for 3 hours. After the reaction was complete, the temperature was lowered to 80°C, and 2.45 g of 30 wt% hydrogen peroxide was added dropwise over approximately 0.5 hours. The reaction was maintained for 2 hours, then cooled to room temperature, and samples were taken for analysis. The results showed that the esterification rate of the product was 93.8%, the content of monophosphate monoester was 79.62%, and the content of diester phosphate was 14.13%.
[0022] Example 2
[0023] 158 g of isomeric decaol, 1.58 g of deionized water, and 0.32 g of liquid catalyst AMC (titanium ester modified) were added to a reaction flask. Stirring was started, and the temperature was raised to 40°C. 87 g of phosphorus pentoxide was then added in batches, maintaining the reaction temperature below 60°C, and the addition was completed in approximately 2 hours. The temperature was then raised to 100°C and maintained for 3 hours. After the reaction was complete, the temperature was lowered to 80°C, and 2.45 g of 30 wt% hydrogen peroxide was added dropwise over approximately 0.5 hours. The reaction was maintained for 2 hours, then cooled to room temperature, and samples were taken for analysis. The results showed that the esterification rate of the product was 93.71%, the content of monophosphate monoester was 82.54%, and the content of diester phosphate was 10.17%.
[0024] Example 3
[0025] 158 g of isomeric decaol, 1.58 g of deionized water, and 1.26 g of liquid catalyst AMC were added to a reaction flask. Stirring was started, and the temperature was raised to 40°C. 87 g of phosphorus pentoxide was then added in batches, maintaining the reaction temperature below 60°C, over approximately 2 hours. The temperature was then raised to 100°C and maintained for 3 hours. After the reaction was complete, the temperature was lowered to 80°C, and 2.45 g of 30 wt% hydrogen peroxide was added dropwise over approximately 0.5 hours. The reaction was maintained for 2 hours, then cooled to room temperature, and samples were taken for analysis. The results showed that the esterification rate of the product was 95.64%, the content of monophosphate monoester was 84.54%, and the content of diester phosphate was 10.27%.
[0026] Example 4
[0027] 158 g of isomeric decaol, 6.32 g of deionized water, and 0.79 g of liquid catalyst AMC were added to a reaction flask. Stirring was started, and the temperature was raised to 40°C. 87 g of phosphorus pentoxide was then added in batches, maintaining the reaction temperature below 60°C, over approximately 2 hours. The temperature was then raised to 100°C and maintained for 3 hours. After the reaction was complete, the temperature was lowered to 80°C, and 2.45 g of 30 wt% hydrogen peroxide was added dropwise over approximately 0.5 hours. The reaction was maintained for 2 hours, then cooled to room temperature, and samples were taken for analysis. The results showed that the esterification rate of the product was 82.64%, the content of monophosphate monoester was 74.54%, and the content of diester phosphate was 6.27%.
[0028] Example 5
[0029] 158 g of isomeric decaol, 3.16 g of deionized water, and 0.79 g of liquid catalyst AMC were added to a reaction flask. Stirring was started, and the temperature was raised to 40°C. 64.3 g of phosphorus pentoxide was then added in batches, maintaining the reaction temperature below 60°C, and the addition was completed in approximately 2 hours. The temperature was then raised to 100°C and maintained for 3 hours. After the reaction was complete, the temperature was lowered to 80°C, and 2.45 g of 30 wt% hydrogen peroxide was added dropwise over approximately 0.5 hours. The reaction was maintained for 2 hours, then cooled to room temperature, and samples were taken for analysis. The results showed that the esterification rate of the product was 95.07%, the content of monophosphate monoester was 83.50%, and the content of diester phosphate was 13.83%.
[0030] Example 6
[0031] 158 g of isomeric decaol, 3.16 g of deionized water, and 0.79 g of liquid catalyst AMC were added to a reaction flask. Stirring was started, and the temperature was raised to 40°C. 70.5 g of phosphorus pentoxide was then added in batches, maintaining the reaction temperature below 60°C, and the addition was completed in approximately 1 hour. The temperature was then raised to 90°C and maintained for 3 hours. After the reaction was complete, the temperature was lowered to 80°C, and 7.11 g of 30 wt% hydrogen peroxide was added dropwise over approximately 1 hour. The reaction was maintained for 2 hours, then cooled to room temperature, and samples were taken for analysis. The results showed that the esterification rate of the product was 91.34%, the content of monophosphate monoester was 84.13%, and the content of diester phosphate was 9.65%.
[0032] Example 7
[0033] 158 g of isomeric decaol, 3.16 g of deionized water, and 0.79 g of liquid catalyst AMC were added to a reaction flask. Stirring was started, and the temperature was raised to 40°C. 75.9 g of phosphorus pentoxide was then added in portions, maintaining the reaction temperature below 60°C, completing the addition in approximately 1 hour. The temperature was then raised to 85°C and maintained for 5 hours. After the reaction was complete, the temperature was lowered to 80°C, and 4.74 g of 30 wt% hydrogen peroxide was added dropwise over approximately 1.5 hours. The reaction was maintained for 3 hours, then cooled to room temperature, and samples were taken for analysis. The results showed that the esterification rate of the product was 93.68%, the content of monophosphate monoester was 87.13%, and the content of diester phosphate was 6.17%.
[0034] Example 8
[0035] 158 g of isomeric decaol, 3.16 g of deionized water, and 0.79 g of liquid catalyst AMC were added to a reaction flask. Stirring was started, and the temperature was raised to 40°C. 75.9 g of phosphorus pentoxide was then added in portions, maintaining the reaction temperature below 60°C, completing the addition in approximately 1 hour. The temperature was then raised to 85°C and maintained for 4 hours. After the reaction was complete, the temperature was lowered to 80°C, and 3.56 g of 30 wt% hydrogen peroxide was added dropwise over approximately 1.5 hours. The reaction was maintained for 3 hours, then cooled to room temperature, and samples were taken for analysis. The results showed that the esterification rate of the product was 94.29%, the content of monophosphate monoester was 88.92%, and the content of diester phosphate was 5.86%.
[0036] Example 9
[0037] 158 g of isomeric decaol, 3.16 g of deionized water, and 0.79 g of liquid catalyst AMC were added to a reaction flask. Stirring was started, and the temperature was raised to 40°C. 75.9 g of phosphorus pentoxide was then added in batches, maintaining the reaction temperature below 60°C, completing the addition in approximately 1 hour. The temperature was then raised to 85°C and maintained for 4 hours. After the reaction was complete, the temperature was lowered to 80°C, and 2.96 g of 30 wt% hydrogen peroxide was added dropwise over approximately 1.5 hours. The reaction was maintained for 3 hours, then cooled to room temperature, and samples were taken for analysis. The results showed that the esterification rate of the product was 95.02%, the content of monophosphate monoester was 90.25%, and the content of diester phosphate was 5.61%.
[0038] Comparative Example 1 158g of isomeric decaol was added to the reaction flask without water or catalyst. Stirring was started, and the temperature was raised to 40°C. 75.9g of phosphorus pentoxide was then added in batches, maintaining the reaction temperature below 60°C, completing the addition in approximately 1 hour. The temperature was then raised to 85°C and maintained for 4 hours. After the reaction was complete, the temperature was lowered to 80°C, and 2.34g of 30wt% hydrogen peroxide was added directly. The reaction was maintained for 2 hours, then cooled to room temperature, and samples were taken for analysis. The results showed that the esterification rate of the product was 92.02%, the content of monophosphate monoester was only 63.29%, while the content of diester phosphate was as high as 33.15%.
[0039] Comparative Example 2 158g of isomeric decaol was added to the reaction flask without water or catalyst. Stirring was started, and the temperature was raised to 40°C. 64.3g of phosphorus pentoxide was then added in batches, maintaining the reaction temperature below 60°C, completing the addition in approximately 1 hour. The temperature was then raised to 85°C and maintained for 4 hours. After the reaction was complete, the temperature was lowered to 80°C, and 2.22g of 30wt% hydrogen peroxide was added directly. The reaction was maintained for 2 hours, then cooled to room temperature, and samples were taken for analysis. The results showed that the esterification rate of the product was 93.44%, the content of monophosphate monoester was only 61.17%, while the content of diester phosphate was as high as 34.68%.
[0040] Comparative Example 3 158 g of isomeric decaol and 3.16 g of deionized water were added to the reaction flask without a catalyst. Stirring was started, and the temperature was raised to 40°C. 75.9 g of phosphorus pentoxide was added in batches, maintaining the reaction temperature below 60°C, and the addition was completed in approximately 1 hour. The temperature was then raised to 85°C and maintained for 4 hours. After the reaction was complete, the temperature was lowered to 80°C, and 2.96 g of 30 wt% hydrogen peroxide was added directly. The reaction was maintained for 2 hours, then cooled to room temperature, and samples were taken for analysis. The results showed that the esterification rate of the product was 88.41%, the content of monophosphate monoester was only 69.24%, and the content of diester phosphate was as high as 18.41%.
[0041] Comparative Example 4 158g of isomeric decaol was added to the reaction flask without water, along with 0.79g of liquid catalyst AMC. Stirring was started, and the temperature was raised to 40°C. 75.9g of phosphorus pentoxide was then added in batches, maintaining the reaction temperature below 60°C, completing the addition in approximately 1 hour. The temperature was then raised to 85°C and maintained for 4 hours. After the reaction was complete, the temperature was lowered to 80°C, and 2.96g of 30wt% hydrogen peroxide was added directly. The reaction was maintained for 2 hours, then cooled to room temperature, and samples were taken for analysis. The results showed that the esterification rate of the product was 94.13%, the content of monophosphate monoester was only 64.47%, while the content of diester phosphate was as high as 33.27%.
[0042] Table 1 shows the main process parameters, esterification rate, and component content of the products in Examples 1-9 and Comparative Examples 1-4.
[0043] In this invention, the amount of water added is precisely controlled within 1%-4% of the isomeric alcohol mass. Within this range, water molecules preferentially attack the P=O bridging bonds of phosphorus pentoxide, depolymerizing it into intermediates of moderately reactive metaphosphoric acid (HPO3) or pyrophosphoric acid (H4P2O7). These intermediates have different steric hindrance and electron cloud density distributions than phosphorus pentoxide. This pre-conversion effectively blocks the pathway for the two active P=O bonds within the phosphorus pentoxide molecule to react simultaneously with the alcohol hydroxyl group, thereby inhibiting diester formation at its source.
[0044] If the water content is too low (<1%), phosphorus pentoxide depolymerization is insufficient, and highly active P4O remains. 10 Clusters lead to a surge in diester content (Comparative Examples 1-2); if the water content is too high (>4%), the excess water will directly react with phosphorus pentoxide to generate orthophosphoric acid (H3PO4), resulting in an increase in the free acid content in the system and a significant decrease in the esterification rate (see Example 4).
[0045] The solid catalyst FEC (zirconia-modified) has abundant Lewis acid sites, and its unique Zr-O bonds can form coordination intermediates with phosphorus pentoxide (Zr on the surface). 4+ The site can specifically adsorb metaphosphoric acid, reducing the activation energy of the esterification reaction, while its rigid framework structure restricts the spatial coupling of the diester; the liquid catalyst AMC (titanium ester modified, Ti-O bond can polarize alcohol hydroxyl groups) in the liquid phase via Ti 4+ The coordination effect of the alcohol hydroxyl group directionally guides the attack of the phosphorus atom of the metaphosphoric acid, significantly improving the monoester selectivity. In other words, both accelerate the monoester formation kinetics by lowering the transition state energy barrier.
[0046] Experiments show that when using unmodified common zirconium oxide or titanate, the monoester content of the product is generally lower than 75%, proving that the modified catalyst plays an irreplaceable role in achieving high monoester content (>90%).
[0047] In the post-treatment stage, the hydrogen peroxide is added dropwise over a period of 0.5-2 hours, preferably 1.5 hours. This design aims to match the decomposition rate of hydrogen peroxide with the hydrolysis rate of the diester. If added all at once (as in Comparative Example 1), the locally high concentration of hydrogen peroxide will cause violent decomposition and exothermic reaction, leading to excessive hydrolysis of some monoesters into orthophosphoric acid, which would reduce the yield. By using a dropwise addition method, the trace amounts of water and reactive oxygen species generated during decomposition are used to gently promote the conversion of residual diesters into monoesters, while simultaneously oxidizing and destroying chromophores, achieving simultaneous "monoester enrichment" and "decolorization". That is, the in-situ water generated by the decomposition of hydrogen peroxide is used to gently hydrolyze the very small amount of diester in the system, rather than directly diluting it, thereby further increasing the monoester content to over 90% while decolorizing.
[0048] Application performance verification: The high monoester content (90.25%) product obtained in Example 9 was compared with a commercially available ordinary phosphate ester with a monoester content of 65%. The product was tested in hard water (Ca... 2+ In an environment of 500 ppm, the emulsion stability of the product of this invention (no precipitation after 24 hours) is significantly better than that of ordinary products; in an alkaline metal processing fluid with pH=9, the corrosion inhibition rate of the product of this invention is increased by more than 30%, which fully verifies the performance leap brought about by the high monoester content.
[0049] To demonstrate that this invention does not simply produce a mixture with a high monoester content, but rather that its physicochemical properties undergo a qualitative change, a comparative sample is prepared: a commercially available high-purity diester phosphate (content >95%) is physically mixed with the product of Example 9 of this invention at a diester:monoester ratio of 5.6:90.3, so that its composition is completely identical to that of the product of Example 9 (referred to as the "physical mixture"). The emulsification stability of the two in hard water (500 ppm Ca) is compared. 2+ ): Product of Example 9 of the present invention: After the emulsion was left to stand for 48 hours, no stratification or precipitation was observed, and the particle size distribution was uniform.
[0050] Physical mixture: After the emulsion was left for 2 hours, an oily precipitate appeared on the surface, and after 4 hours, it clearly separated into layers.
[0051] The comparative results strongly demonstrate that in the products obtained by the present invention through a specific synthetic route (preconversion of water and phosphorus pentoxide → directional esterification by catalyst → dynamic hydrolysis of hydrogen peroxide), the monoesters and diesters (and possibly other components) form a specific intermolecular arrangement or association structure. This "in-situ generated" structure endows the products with macroscopic properties far exceeding the simple summation of its components.
[0052] The above embodiments of the present invention provide a method for synthesizing isomeric alcohol phosphate monoesters, which has the following main advantages: 1) This invention, through the synergistic effect of catalytic esterification and hydrolysis processes, can stably produce high-purity products with an esterification rate >95% and a monophosphate content >90%. Compared to conventional phosphate ester products on the market (where the mono- and diester ratio is typically 1:1 and the monoester content is generally <70%), the product of this invention achieves a breakthrough improvement in hydrophilicity, emulsification, and wetting properties, and can meet the stringent requirements for high-performance anionic surfactants in fields such as metalworking fluids and high-end pesticide formulations.
[0053] 2) Traditional processes, in order to obtain high-content monoesters, typically require the use of the highly hazardous chemical phosphorus oxychloride as a raw material. The reaction process generates a large amount of hydrogen chloride gas, causing severe corrosion to equipment and necessitating specialized corrosion-resistant equipment. This invention eliminates the use of phosphorus oxychloride, instead using phosphorus pentoxide and water as raw materials. The reaction process is mild and safe, producing no highly corrosive gases, significantly reducing the material requirements for production equipment and substantially lowering safety risks and environmental treatment costs.
[0054] 3) This invention innovatively introduces a synergistic regulation mechanism between water and a specific catalyst (FEC / AMC): the water added to the reaction system can pre-convert the highly active phosphorus pentoxide into metaphosphoric acid and / or pyrophosphoric acid, effectively regulating the activity of the reaction sites and preventing phosphorus pentoxide from directly reacting with the two hydroxyl groups of the isomeric alcohol to form a diester, thereby inhibiting the formation of byproducts from the source. The zirconium oxide or titanate modified catalyst used not only accelerates the esterification reaction rate but also effectively inhibits the excessive hydrolysis of the already formed phosphate monoester during hydrolysis, ensuring the stability of the product structure.
[0055] 4) In the post-processing stage, this invention uses hydrogen peroxide for hydrolysis and decolorization: its strong oxidizing properties destroy the conjugated system, effectively removing chromogenic groups from the product and significantly improving the product's appearance and color. The active oxygen and water generated by the decomposition of hydrogen peroxide provide hydrolysis raw materials for the small amount of residual diester phosphate in the system, promoting the further conversion of diester into monoester, and further increasing the monoester content and esterification rate of the product.
[0056] In summary, this invention ensures that the product has excellent surface activity while achieving a safe, green, and low-cost production process, thus possessing extremely high industrial application value and broad market prospects.
[0057] The above are merely preferred embodiments of the present invention. It should be noted that those skilled in the art can make several modifications and improvements without departing from the concept of the present invention, and these should also be considered within the scope of protection of the present invention. These will not affect the effectiveness of the implementation of the present invention or the practicality of the patent.
Claims
1. A method for synthesizing isomeric alcohol phosphate monoesters, characterized in that, Includes the following steps: Add isomeric alcohol, catalyst and water to the reaction vessel, add phosphorus pentoxide while controlling the temperature at 40-60℃, and after the addition is complete, raise the temperature to 80-100℃ to carry out the esterification reaction and keep the reaction at the temperature for 3-5 hours. After the reaction is complete, cool the temperature to 70-90℃ and add hydrogen peroxide for hydrolysis and decolorization treatment to obtain isomeric alcohol phosphate monoester; The molar ratio of the isomeric alcohol to phosphorus pentoxide is 1.7-2.3:
1. The amount of catalyst used is 0.2%-0.8% of the mass of the isomeric alcohol; The amount of water added is 1%-4% of the mass of the isomeric alcohol; The amount of hydrogen peroxide added is 1%-3% of the total material mass.
2. The method for synthesizing isomeric alcohol phosphate monoesters according to claim 1, characterized in that, The molar ratio of the isomeric alcohol to phosphorus pentoxide is 1.9-2.0:1; The amount of catalyst used is 0.5%-0.6% of the mass of the isomeric alcohol; The amount of water added is 2%-2.5% of the mass of the isomeric alcohol.
3. The method for synthesizing isomeric alcohol phosphate monoesters according to claim 1, characterized in that, The phosphorus pentoxide is added at a time of 0.5-2 hours.
4. The method for synthesizing isomeric alcohol phosphate monoesters according to claim 3, characterized in that, The esterification reaction was carried out at a temperature of 85°C for 4 hours.
5. The method for synthesizing isomeric alcohol phosphate monoesters according to claim 1, characterized in that, The catalyst is selected from at least one of solid catalyst FEC or liquid catalyst AMC; Wherein, FEC is a zirconium oxide modified compound, and AMC is a titanate modified compound.
6. The method for synthesizing isomeric alcohol phosphate monoesters according to claim 5, characterized in that, The catalyst is a liquid catalyst, AMC.
7. The method for synthesizing isomeric alcohol phosphate monoesters according to claim 1, characterized in that, The hydrogen peroxide is added over a period of 0.5-2 hours, and the hydrolysis time is 2-4 hours. The temperature for hydrolysis and decolorization is 70-90℃.
8. The method for synthesizing isomeric alcohol phosphate monoesters according to claim 7, characterized in that, The amount of hydrogen peroxide added is 1.25% of the total material mass, the dripping time is 1.5h, the hydrolysis time is 3h, and the hydrolysis temperature is 80℃.
9. The method for synthesizing isomeric alcohol phosphate monoesters according to claim 1, characterized in that, The addition of water is used to regulate the reaction system and convert phosphorus pentoxide into metaphosphoric acid and / or pyrophosphoric acid to directionally inhibit the formation of phosphate diesters. The hydrogen peroxide not only acts as a decolorizing agent, but also participates in the reaction with the active oxygen and water generated during its hydrolysis, inhibiting the excessive hydrolysis of phosphate monoesters and improving the color of the product.
10. The method for synthesizing isomeric alcohol phosphate monoesters according to claim 1, characterized in that, The product obtained by the method has an esterification rate of greater than 95% and a phosphate monoester content of greater than 90%.