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Thiopolyphosphate as well as preparation method and application thereof

A technology of thiopolyphosphate and polyphosphate, applied in the field of polymer materials, can solve the problems of affecting the degradation process and speeding up the degradation of polyphosphates

Active Publication Date: 2020-09-22
合肥阿法纳生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, Professor Wang Jun's research group found that polyphosphate esters substituted with side group amino groups will greatly accelerate the degradation of polyphosphate esters, and different amino side chains will also affect the degradation process.

Method used

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  • Thiopolyphosphate as well as preparation method and application thereof
  • Thiopolyphosphate as well as preparation method and application thereof
  • Thiopolyphosphate as well as preparation method and application thereof

Examples

Experimental program
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Effect test

preparation example Construction

[0075] The present invention also provides a preparation method of polythiophosphate, comprising: mixing and reacting the phosphorothioate monomer shown in formula (III), initiator and catalyst under anhydrous conditions to obtain ) structure of thiopolyphosphate; wherein, the initiator is a polymer compound initiator with a hydroxyl group at the end, a polylactone compound with a hydroxyl group at the end, a small molecular compound initiator containing a hydroxyl group or a small molecule compound containing a hydroxyl salt Molecular compound initiator;

[0076] Or polymerize the monomer represented by formula (II) to obtain polythiophosphate;

[0077]

[0078] Among them, R 1 It is the residue after one hydroxyl group is removed from a polymer compound with a hydroxyl group at the end, the residue after one hydroxyl group is removed from a hydroxyl-containing small molecule compound, or the residue after one hydroxyl group is removed from a polylactone compound; R 2 is...

Embodiment 1

[0104] Embodiment 1: Oxyphosphoryl chloride CTP is the synthesis of the compound shown in formula (V)

[0105]

[0106] All reactants were purified by vacuum distillation before the reaction started. The reaction needs to be carried out under anhydrous conditions, and phosphorus trichloride is dissolved in anhydrous dichloromethane to keep the reactant concentration at 1.0mol / L, constantly stir at room temperature, then slowly add dropwise the dichloromethane solution of ethylene glycol ( 1.0mol / L), wherein the molar ratio of phosphorus oxychloride to ethylene glycol is 1:1, and the HCI generated by the reaction is absorbed in time with solid sodium hydroxide. After 6 hours, the reaction was completed, and the solvent was removed by a rotary vane vacuum pump, and purified by distillation under reduced pressure to obtain cyclic trivalent phosphorus oxychloride as a colorless clear liquid with a pungent smell. Dissolve cyclic trivalent phosphorus oxychloride in anhydrous ben...

Embodiment 2

[0108] Embodiment 2: the synthesis of phosphorothioate monomer

[0109]

[0110] R:-CH 3 -CH 2 CH 3 -CH 2 CH 2 CH 3 -CH 2 CH 2 CH 2 CH 3 -CH 2 CH 2 CH 2 CH 2 CH 3 -CH 2 CH 2 CH 2 CH 2 CH 2 CH 3

[0111] Before the reaction starts, the reactants and the solvent are all dried. The reaction must be carried out under anhydrous conditions, and the device is a three-necked flask containing a constant pressure dropping funnel, and the molar ratio is acid chloride:alcohol:triethylamine=1:1:1. Utilize heating and vacuum condition to remove a small amount of water contained in the reaction device, the concrete reaction is as follows:

[0112] First add anhydrous tetrahydrofuran to the three-necked flask, and then add methyl mercaptan to keep its concentration at 1.0 mol / L. Add triethylamine therein again, drop the compound shown in formula (V) to reaction device through dropping funnel. The reaction was carried out at 0°C for 10 h, and a white precipitate...

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Abstract

The invention provides thiopolyphosphate. The thiopolyphosphate comprises a structure shown in a formula (I) or is obtained by polymerizing a monomer shown in a formula (II). Compared with the prior art, the thiopolyphosphate provided by the invention has good hydrophobicity, decomposition resistance and hydrogen peroxide specific degradability, and can be used as an environmental response degradable material.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a thiopolyphosphate, its preparation method and application. Background technique [0002] Polyphosphoester is a new type of degradable material that has developed rapidly in recent years. Unlike polyesters, which have carbonate bonds as their linking structure, it uses phosphate bonds as their main chain linking structure. Phosphate bonds can be slowly degraded in physiological environments, and the structure of polyphosphates is variable, so it is easy to carry out functional modification on side groups. [0003] The structure of polyphosphate has the following advantages: (1) The chemical structure is changeable and the properties can be adjusted. The R group of the main chain can be changed by changing the type of initiator, and many properties of the polyphosphate can be regulated by changing the R' group of the side chain of the phosphate monomer; T...

Claims

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Application Information

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IPC IPC(8): C08G79/04
CPCC08G79/04
Inventor 王育才刘懿樊峰
Owner 合肥阿法纳生物科技有限公司
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