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A method for increasing the molecular weight and yield of polyphosphazene elastomer

An elastomer and polyphosphazene technology is applied in the field of preparation of improving the molecular weight of elastomer products, can solve problems such as low molecular weight and low yield, and achieve the effects of reducing impact, avoiding raw material waste, and saving raw material costs

Active Publication Date: 2021-04-02
山东航橡新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention is for the preparation of polyphosphazene elastomer, provides a kind of synthetic method that improves the ring-opening polymerization yield of cyclic phosphazene and product molecular weight, solves the problem of low yield and low molecular weight in the traditional synthetic method, and saves raw materials cost, suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032]Add 1000ml of 1,4-dioxane into a 2000ml three-necked flask, and add 58g of sodium to the solvent. The system needs to be connected to a condensation system. A solution of about 250g of mixed phenol and 250ml of 1,4-dioxane in equimolar amounts was slowly added dropwise to the sodium-containing flask, and 10% excess phenol was added to the system to ensure that all the sodium was completely reacted. Wait until the reaction is complete, that is, all the sodium blocks disappear, and the sodium phenol salt solution is obtained, which is sealed for use.

[0033] The preparation of the activating agent of PDCP polymerization, the PDCP of 80% phenoxyl substitution rate is to first synthesize PDCP by the method reported in the literature of Joseph H.Magill, or the PDCP that obtains separation in step (2), utilize 1.1 times of equivalent again Sodium phenoxide was refluxed with THF as a solvent for 24 hours to perform substitution to prepare PDCP with 80% phenoxy substitution rat...

Embodiment 2

[0036] Add 1000ml of pyridine to a 2000ml three-necked flask, and add 58g of sodium to the solvent. The system needs to be connected to a condensation system. About 250g of equimolar amounts of mixed phenol and 250ml of pyridine are made into a solution and slowly added dropwise to the sodium-containing flask, and 10% excess phenol is added to the system to ensure that all sodium is completely reacted. Wait until the reaction is complete, that is, all the sodium blocks disappear, and the sodium phenol salt solution is obtained, which is sealed for use.

[0037] The preparation of the active agent of PDCP polymerization, the PDCP of 30% ethoxyl substitution rate is to first synthesize PDCP by the method reported in the literature of Joseph H.Magill, and then use 0.5 times the equivalent of sodium ethoxide to THF as the solvent ice bath for 24h, carry out Substitution to prepare PDCP with 30% ethoxyl substitution.

[0038] Get 120g monomer hexachlorocyclotriphosphazene, 50gPCl ...

Embodiment 3

[0040] Add 1000ml of acetonitrile into a 2000ml three-neck flask, add 58g of sodium to the solvent, and the system needs to be connected to a condensation system. About 250g of phenol and 250ml of acetonitrile of equimolar amount are dubbed into the solution slowly dropwise into the sodium-containing flask, and 10% excess phenol is added to the system to ensure that all the sodium is completely reacted. Wait until the reaction is complete, that is, all the sodium blocks disappear, and the sodium phenol salt solution is obtained, which is sealed for use.

[0041] The preparation of the concentrated solution is through the synthesis of PDCP method reported in the literature of Joseph H.Magill or the polymerization process in step (1), after the PDCP polymerization reaction is completed, the temperature is down to room temperature, and the reaction solution is filtered or precipitated or extracted. A combination of one or more technical means is used to separate high polymers fro...

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Abstract

The invention discloses a method for improving the molecular weight and the yield of a polyphosphazene elastomer, and belongs to the technical field of preparation of polyphosphazene elastomers. The method comprises the following steps: (1) adding a high-boiling-point solvent, reaction raw materials (astarting materialand a hexachlorocyclotriphosphazene monomer), a catalyst, a cocatalyst and an active agent into an anhydrous oxygen-free reaction container, raising the temperature of the system under stirring to 170-250 DEG C, and carrying out a constant-temperature reaction for 0.5-10 hours; then, supplementing an organic solvent or a precipitant into the system, adjusting the reaction temperature to continuously react for 1-30 hours, separating and extracting the reacted PDCP polymer after the reaction is finished, and concentrating the rest of the mixed solution containing a small part of PDCP and a monomer; and (3) adding the PDCP solution obtained in the step (2) into a mixture containing a substitution reagent, an acid-binding agent and a solvent, and performing a reaction, so as to obtain the completely substituted polyphosphazene elastomer. The relative molecular mass of thepolyphosphazene elastomer is improved, and meanwhile, the yield and the solvent utilization rate are increased.

Description

technical field [0001] The invention relates to the technical field of polyphosphazene elastomer preparation, in particular to a preparation method suitable for engineering, capable of greatly increasing yield, reducing cost and increasing the molecular weight of elastomer products. Background technique [0002] Polyphosphazene elastomer is a new type of inorganic-organic high polymer with P and N double bonds alternately arranged as the main chain structure. The diversity of side group structures can generate a variety of derivatives, which can have good water resistance and oil resistance. , high temperature resistance, low temperature resistance and non-combustibility and other comprehensive excellent properties. [0003] The difficulty of preparation of functional polyphosphazene materials has limited the development of its large-scale application. Long-term research has also been devoted to the development of economical, efficient and convenient polymerization processes...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G79/025
CPCC08G79/025
Inventor 吴战鹏张双琨赵静存刘伟武德珍张立群邹文奇苗振威
Owner 山东航橡新材料有限公司
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