A kind of method and application thereof for preparing didecyl calcium phosphate
A technology of didecyl calcium phosphate and didecyl phosphoric acid, which is applied in the field of electrochemistry, can solve the problems of complex preparation methods of calcium salts, unfavorable promotion and application of calcium ion selective electrodes, and achieve high yield, low cost, and high production efficiency. The effect of simple method
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[0031] The preparation of present embodiment didecyl calcium phosphate is based on following principle:
[0032] 1) Decanol and phosphorus oxychloride generate oxidized didecyl phosphate in the presence of pyridine;
[0033]
[0034] 2) Oxidized didecyl phosphate is then hydrolyzed and acidified to generate didecyl phosphoric acid;
[0035]
[0036] 3) Didecyl Phosphate and Saturated CaCl 2 React at 40°C to generate didecyl calcium phosphate.
[0037] 2(C 10 h 23 O) 2 POOH+CaCl 2 →[(C 10 h 23 O) 2 POO] 2 Ca↓+2HCl
[0038] In step 1), the volume ratio of the reaction substrates decanol and phosphorus oxychloride in the embodiment of the present invention is 2:1; decyl alcohol is 100 mL, and phosphorus oxychloride is 50 mL.
[0039] In the embodiment of the present invention, the volume ratio of the reactants decyl alcohol, phosphorus oxychloride and pyridine is 2:1:2.
[0040] In the embodiment of the present invention, the reactant and the catalyst are reacte...
Embodiment 1 2
[0051] The synthesis of embodiment 1 didecyl phosphoric acid
[0052] 1. Raw material
[0053] ① ether: use anhydrous Na 2 SO 4 dehydration
[0054] ②Pyridine: dehydrated with anhydrous KOH
[0055] ③ Phosphorus oxychloride: dehydrated with anhydrous KOH
[0056] ④Decanol: Dehydration with anhydrous NaOH
[0057] 2. Instrument return device
[0058] 3. Steps
[0059] 1) Synthesis of oxidized didecyl phosphate:
[0060] ①POCl3 (50mL) into the round bottom flask of the reflux device, then add 500mL of ether, and stir;
[0061] ②Decanol (100mL) dissolved in ether;
[0062] ③Pyridine (100mL) dissolved in ether;
[0063] ④In the stirring state, adjust the speed to about 90±10 rpm, and slowly drop the ether solution of decyl alcohol into the round bottom flask from the dropping funnel, and control the dropping speed to 30-40 drops / min;
[0064] ⑤ Slowly drop the ether solution of pyridine into the flask at 60 drops / min;
[0065] ⑥ After the dropwise addition, react at ro...
Embodiment 2 2
[0076] Identification of embodiment 2 didecyl phosphate
[0077] 1. Detection methods and conditions
[0078] In this example, four detection methods are used to detect the product after the synthesis reaction in Example 1 is completed. Due to the fragmentation process of the substance in the mass spectrometer, different molecular ion peaks or fragment ion peaks of positive and negative ions are generated. The positive ion mode of the mass spectrometer can only detect positively charged ion fragments, while the negative ion mode can only detect negative ions. The first three detection methods scan ions from different sides to analyze the product comprehensively and select the appropriate mass spectrometry conditions. The fourth type adds mass spectrometry (MS) to liquid chromatography (LC), which can separate and measure various components in the product, and the analysis accuracy and sensitivity are higher. Tridecyl phosphate is a by-product of the synthesis reaction.
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