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Phosphate-pyrimidine zinc dichloride complex with catalytic performance as well as preparation method and application of phosphate-pyrimidine zinc dichloride complex

A technology of zinc pyrimidine dichloride, catalytic performance, applied in the direction of organic compound/hydride/coordination complex catalyst, organic chemical method, zinc organic compound, etc., can solve the trouble of removing anti-gelling agent and low grafting rate And other issues

Active Publication Date: 2020-07-07
JIANGSU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] "Research on Maleic Anhydride Grafted Liquid Polybutadiene" (Anhui Chemical Industry, 1998,93 (3): 32-34), "Measuring Method of Maleic Anhydride Grafted Liquid Isoprene Rubber Grafting Rate" (high function Acta Molecule Sinica, 2015, 28 (4): 398-402) discloses that liquid polybutadiene, liquid polyisoprene and maleic anhydride are grafted, and this reaction generally adopts thermal initiation and initiator to initiate free radicals to carry out Grafting reaction, that is, grafting reaction needs to occur under the conditions of high temperature 180-220 ℃ and BPO and other initiators. The grafting rate of this method can reach more than 7%. On the one hand, the higher the reaction temperature is, the higher the grafting rate is, but The higher the temperature, the more likely to be glued between the raw materials during the reaction process, so generally more anti-gelling agents need to be added during the reaction process. If the temperature of the grafting reaction is lowered, a large amount of monomers will remain and the grafting rate will be lower. Low, the addition of anti-gelling agent will bring additional production cost to the product, and it will also bring great trouble to remove the anti-gelling agent in the later separation and purification

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  • Phosphate-pyrimidine zinc dichloride complex with catalytic performance as well as preparation method and application of phosphate-pyrimidine zinc dichloride complex
  • Phosphate-pyrimidine zinc dichloride complex with catalytic performance as well as preparation method and application of phosphate-pyrimidine zinc dichloride complex
  • Phosphate-pyrimidine zinc dichloride complex with catalytic performance as well as preparation method and application of phosphate-pyrimidine zinc dichloride complex

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preparation example Construction

[0034] The second aspect of the embodiments of the present invention provides a method for preparing a phosphoric acid-pyrimidine zinc dichloride complex with catalytic properties, comprising the following steps:

[0035] (1) Synthesis of organic ligand pyrimidine-2 phosphate dimethyl:

[0036]

[0037] Dissolving 2-bromopyrimidine as shown in the structure of formula I in an amide solvent to form a 2-bromopyrimidine solution;

[0038] Suspend sodium hydride in an amide solvent to form a sodium hydride suspension, add dimethyl phosphite to the sodium hydride suspension, stir for reaction, then add the 2-bromopyrimidine solution, heat up the reaction, and wait for the reaction After the end, concentrate under reduced pressure to remove the amide solvent to form a concentrate, add ice water to the concentrate, extract the water phase, combine the organic phase, wash, dry, and concentrate the organic phase to obtain a crude product, purify Process to obtain pyrimidine-2-phosp...

Embodiment 1

[0052] A method for preparing a phosphoric acid-pyrimidine zinc dichloride complex with catalytic performance, comprising the steps of:

[0053] (1) Synthesis of organic ligand pyrimidine-2 phosphate dimethyl:

[0054]

[0055] In a container equipped with magnetic stirring, 4.0g (100mmol) sodium hydride (commercial reagent, sodium hydride dispersed in mineral oil, sodium hydride content in 60wt%) was suspended in 200mL of anhydrous dimethylacetamide ( DMAc) solvent to form a sodium hydride suspension, then slowly add a DMAc solution (10 mL) of 11 g (100 mmol) dimethyl phosphite (CAS No. 868-85-9) into the sodium hydride suspension under stirring, and add After completion, the reaction was stirred at room temperature for 0.5h; then 15.8g (100mmol) of 2-bromopyrimidine in DMAc (50mL) as shown in the structure of formula I was added to the above reaction system, and then the temperature was raised to 160°C for 24h; the reaction ended Finally, the oil pump concentrated under ...

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Abstract

The invention relates to a phosphoric acid-pyrimidine zinc dichloride complex with catalytic performance and a preparation method and an application thereof, the molecular formula of the phosphoric acid-pyrimidine zinc dichloride complex is C12H18Cl2N4O6P2Zn, the phosphoric acid-pyrimidine zinc dichloride complex is a monoclinic system, and a space group of the phosphoric acid-pyrimidine zinc dichloride complex is P212121; the preparation method comprises the following steps: synthesizing an organic ligand by taking 2-bromopyrimidine and dimethyl phosphite as raw materials, and coordinating the ligand with zinc dichloride to prepare a phosphoric acid-pyrimidine zinc dichloride complex. When the complex is used as a catalyst to catalyze a grafting reaction of diene liquid rubber and maleicanhydride, the reaction temperature in the reaction process can be effectively reduced, the probability of gelation in the grafting reaction process is extremely low, the catalytic grafting efficiencyis higher, and the grafting rate of the grafted product reaches 15-20%.

Description

technical field [0001] The invention relates to the technical field of synthesis and application of transition metal complexes, in particular to a phosphoric acid-pyrimidine zinc dichloride complex with catalytic performance and its preparation method and application. Background technique [0002] Pyrimidine-phosphate compounds contain not only the nitrogen atom of pyrimidine, but also the phosphorus and oxygen atoms of phosphoric acid group, so they can easily form metal complexes with special three-dimensional structures with transition metal ions. Moreover, the nitrogen atom of pyrimidine and the oxygen atom of phosphoric acid can be used as good recognition groups for hydrogen bonds, which is conducive to the activation of some active compounds (such as phenols, acid anhydrides, amines, etc.) These compounds undergo important chemical reactions such as addition, substitution, and polymerization. [0003] Liquid rubber is a new low-molecular-weight liquid material with a...

Claims

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Application Information

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IPC IPC(8): C07F3/06B01J31/22C08F279/02C08F222/06C08F4/50
CPCC07F3/003B01J31/2217C08F279/02C08F4/50C07B2200/13B01J2531/26B01J2531/0213C08F222/06
Inventor 罗世鹏陶紫薇李直坤王欣杨廷海
Owner JIANGSU UNIV OF TECH
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