Silicon-based phosphate and preparation method thereof

A technology of silicon-based phosphate ester and inorganic phosphate, which is applied in the direction of phosphorus organic compounds, can solve the problems of harming the body and the environment, corroding equipment, cumbersome preparation methods, etc., and meets the requirements of industrial production, low cost, and safe and easy-to-obtain raw materials Effect

Pending Publication Date: 2022-05-13
JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method still introduces halogen when preparing intermediates, and there is a problem of generating halogen salts, and this method needs to be carried out in an organic solvent, which has problems such as corrosion of equipment and harm to the body and the environment, and the use of toxic solvents also has safety problems. risk
In addition, this method is a multi-step reaction, and steps such as separation of intermediates and removal of organic solvents are required, and the preparation method is still relatively cumbersome.

Method used

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  • Silicon-based phosphate and preparation method thereof
  • Silicon-based phosphate and preparation method thereof
  • Silicon-based phosphate and preparation method thereof

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preparation example Construction

[0044] The invention provides a method for preparing silicon-based phosphate, comprising the steps of:

[0045] Mixing disilazane compound, cyclic internal amine compound A and organic base for pre-reaction, then adding inorganic phosphate, and mixing reaction to prepare silicon-based phosphate;

[0046] Disilazane compounds have a structure shown in the following formula (I):

[0047]

[0048] Among them, R 1 ~R 3 Each occurrence is independently selected from H, F, substituted or unsubstituted alkyl, substituted or unsubstituted alkoxy, substituted or unsubstituted unsaturated hydrocarbyl, or substituted or unsubstituted aromatic hydrocarbyl;

[0049] Cyclic internal amine compound A is selected from One of.

[0050] The present invention uses disilazane compounds as raw materials, which are cheap, but are easily hydrolyzed under neutral or acidic conditions. In the present invention, by adding an organic base to the reactant, on the one hand, the organic base can...

Embodiment 1

[0097] This embodiment provides a preparation method of silicon-based phosphate, the steps are as follows:

[0098] (1) Hydrogenate 2,5-dihydropyrrole (2.0mol), 1,3-divinyl-1,1,3,3-tetramethyldisilazane (1.5mol) and Sodium (0.3mol) was mixed, stirred and reacted for 3h, and the reaction temperature was kept at 20°C to continue the reaction;

[0099] (2) After almost no ammonia gas is produced, the temperature is raised, ammonia gas is evaporated at normal pressure and 60°C, and the temperature is kept constant, and ammonium dihydrogen phosphate (0.6mol) is added to react for 2.5 hours;

[0100] (3) After the reaction is over, distill under reduced pressure to obtain tris(vinyldimethylsilane) phosphate (0.49mol), with a yield of 81.7% and a purity of 99.65%. The results of GC chromatographic analysis are shown in figure 1 ,Table 1.

[0101] Table 1

[0102]

[0103]

Embodiment 2

[0105] This embodiment provides a preparation method of silicon-based phosphate, the steps are as follows:

[0106] (1) Under the condition of ice-water bath (0~4℃), mix 2,5-dihydropyrrole (2.0mol), 1,3-divinyl-1,1,3,3-tetramethyldisilazide Alkane (1.5mol) and sodium hydride (0.3mol) were mixed, stirred and reacted for 5h;

[0107] (2) After almost no ammonia gas is produced, the temperature is raised, and the ammonia gas is evaporated at normal pressure and 50°C, and the temperature is kept constant, and ammonium dihydrogen phosphate (0.6mol) is added to react for 3 hours;

[0108] (3) After the reaction was completed, tris(vinyldimethylsilane)phosphate (0.50 mol) was obtained by distillation under reduced pressure, with a yield of 83.3% and a purity of 99.71%.

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Abstract

The invention relates to a preparation method of silicon-based phosphate. Comprising the following steps: mixing a disilazane compound, a cyclic amine compound A and an organic alkali, carrying out a pre-reaction, adding an inorganic phosphate, and carrying out a mixed reaction to prepare the silicon-based phosphate, the types of the disilazane compound and the cyclic amine compound A are specifically limited. The disilazane compound and the cyclic amine compound A react with the organic base and the inorganic phosphate to prepare the silicon-based phosphate, separation and purification of an intermediate are not needed in the preparation process, one-pot preparation of the silicon-based phosphate can be achieved, the steps are simple and convenient, the method can be carried out under the solvent-free condition, and the method is suitable for industrial production. The preparation method has the advantages of simple process, convenience in operation, avoidance of harm and subsequent treatment problems caused by the use of an organic solvent, no corrosion to equipment, avoidance of the generation of halogen salts by adopting the disilazane compound, and better avoidance of adverse effects on the performance of the battery.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a silicon-based phosphate and a preparation method thereof. Background technique [0002] In recent years, due to the advantages of high energy density, long cycle life, and no pollution, lithium-ion batteries have very broad application prospects. With the continuous in-depth research on lithium-ion batteries, researchers have found that silicon-based phosphate esters containing P-O-Si bonds are used as additives for lithium-ion battery electrolytes, which can inhibit the reaction of unreacted polymerizable compounds in the electrodes, thereby inhibiting the battery. Resistance increases and capacity reduction can be suppressed. When the non-aqueous electrolyte contains sultone with unsaturated hydrocarbon groups and tris(trimethylsilyl)phosphate, a low-resistance film can be formed on the surface of the negative electrode without reducing the high-current performance...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09
CPCC07F9/09
Inventor 王凯范伟贞信勇赵经纬
Owner JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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