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Method for controlling molecular weight of linear polyphosphazene intermediate

A polyphosphazene and intermediate technology, applied in the field of controllable average molecular weight of linear polyphosphazene intermediates, can solve the problems of unresolved and reported controllable polymerization, and achieve the effect of stable purity

Inactive Publication Date: 2018-07-20
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But all are based on the influence of a single condition change on the activity of the polymerization reaction and the crosslinking of the product, but the controllable polymerization of the molecular weight stability control of the linear polyphosphazene intermediate has not been resolved and reported

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0020] Dissolve 50g of hexachlorocyclotriphosphazene into 40ml of 1,2,4-trichlorobenzene, put the solution into a fully dry reaction kettle, and incorporate nitrogen protection; the catalytic system used is sulfamic acid as a catalyst, CaSO 4 2H 2 O is a synergistic catalyst, the amount of catalyst is 1.2wt% of the monomer mass, CaSO 4 2H 2 The mass ratio of O to sulfamic acid is 1:10; the ring-opening polymerization reaction temperature is controlled at 215°C; when the polymerization solution appears to climb rods, it is the end of the polymerization reaction. The number average molecular weight Mn of preparing linear polyphosphazene intermediate is 1×10 3 -9×10 3 grade.

Embodiment example 2

[0022] Dissolve 50g of hexachlorocyclotriphosphazene into 50ml of 1,2,4-trichlorobenzene, put the solution into a fully dry reaction kettle, and incorporate nitrogen protection; the catalytic system used is sulfamic acid as a catalyst, CaSO 4 2H 2 O is a synergistic catalyst, the amount of catalyst is 1.0wt% of the monomer mass, CaSO 4 2H 2 The mass ratio of O to sulfamic acid is 1:10; the ring-opening polymerization reaction temperature is controlled at 210°C; when the polymerization solution appears to climb rods, it is the end of the polymerization reaction. The number average molecular weight Mn of preparing linear polyphosphazene intermediate is 1×10 4 -9×10 4 grade.

Embodiment example 3

[0024] Dissolve 50g of hexachlorocyclotriphosphazene into 70ml of 1,2,4-trichlorobenzene, put the solution into a fully dry reaction kettle, and incorporate nitrogen protection; the catalytic system used is sulfamic acid as a catalyst, CaSO 4 2H 2 O is a synergistic catalyst, the amount of catalyst is 0.9wt% of the monomer mass, CaSO 4 2H 2 The mass ratio of O to sulfamic acid is 1:10; the ring-opening polymerization reaction temperature is controlled at 208°C; when the polymerization solution appears to climb rods, it is the end of the polymerization reaction. The number average molecular weight Mn of preparing linear polyphosphazene intermediate is 1×10 5 -9×10 5 grade.

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Abstract

The invention discloses a method for controlling the molecular weight of a linear polyphosphazene intermediate. The molecular weight of the linear polyphosphazene intermediate is controllable, and thelinear polyphosphazene intermediate with the specific molecular weight can be prepared according to subsequent substitution reaction requirements or application requirements of a polyphosphazene material. According to the method disclosed by the invention, a catalyst with a specific ratio, specific monomer concentration and specific reaction temperature are utilized to obtain the linear polyphosphazene intermediate with different molecular weights. By adopting a reaction control method, the common problems in an existing method that the control variable is single, control conditions are not comprehensive, the control effect is not stable and the like are solved. According to the method disclosed by the invention, the number average molecular weight of the linear polyphosphazene intermediate is controlled to be in three grades including 1*10<3> to 9*10<3>, 1*10<4> to 9*10<4> and 1*10<5> to 9*10<5>; specific polymerization conditions can be selected according to different substitution requirements or application requirements to prepare the linear polyphosphazene intermediate with the specific molecular weight; the method has important significance on application and production of polyphosphazene.

Description

Technical field: [0001] The invention discloses a method for realizing the controllable average molecular weight of a linear polyphosphazene intermediate in a polymerization process by comprehensively adjusting the initial concentration of a monomer, the amount of a catalyst, and the polymerization temperature. Background technique: [0002] The skeleton of polyphosphazene elastomer is arranged alternately with single and double bonds of P and N inorganic atoms. The P-N bond is long and the bond angle is large. The glass transition temperature and the large bond energy of the P=N bond make the polyphosphazene skeleton have good thermal stability. The side groups of linear polydichlorophosphazene can be replaced by different types of nucleophiles to obtain polyphosphazenes with various functions, which can be used as biomedical materials, high temperature resistant materials, low temperature elastomers, sealing materials, oil transport materials, polymer conductors, etc. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/025
CPCC08G79/025
Inventor 王秀芬赵章启蔡喜梅耿婷婷李双联杨立鹏
Owner BEIJING UNIV OF CHEM TECH
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